CN102643612B - Saponifiable matter extraction method and saponifiable matter extraction device - Google Patents
Saponifiable matter extraction method and saponifiable matter extraction device Download PDFInfo
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- CN102643612B CN102643612B CN 201210122344 CN201210122344A CN102643612B CN 102643612 B CN102643612 B CN 102643612B CN 201210122344 CN201210122344 CN 201210122344 CN 201210122344 A CN201210122344 A CN 201210122344A CN 102643612 B CN102643612 B CN 102643612B
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- black liquor
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- 238000000605 extraction Methods 0.000 title abstract description 38
- 238000000034 method Methods 0.000 claims abstract description 35
- 238000000926 separation method Methods 0.000 claims abstract description 18
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims abstract description 8
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 8
- 239000011734 sodium Substances 0.000 claims abstract description 8
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 claims abstract description 5
- 239000004094 surface-active agent Substances 0.000 claims abstract description 5
- 239000007787 solid Substances 0.000 claims description 12
- 239000013543 active substance Substances 0.000 claims description 11
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 7
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 7
- 235000011152 sodium sulphate Nutrition 0.000 claims description 7
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 5
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 4
- -1 ether carboxylate Chemical class 0.000 claims description 4
- 150000002191 fatty alcohols Chemical class 0.000 claims description 4
- 238000009434 installation Methods 0.000 claims description 4
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 4
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 4
- 229920001184 polypeptide Polymers 0.000 claims description 4
- 102000004196 processed proteins & peptides Human genes 0.000 claims description 4
- 108090000765 processed proteins & peptides Proteins 0.000 claims description 4
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 4
- 239000004711 α-olefin Chemical group 0.000 claims description 4
- DNIAPMSPPWPWGF-GSVOUGTGSA-N (R)-(-)-Propylene glycol Chemical compound C[C@@H](O)CO DNIAPMSPPWPWGF-GSVOUGTGSA-N 0.000 claims description 3
- 241001122767 Theaceae Species 0.000 claims description 3
- 125000005227 alkyl sulfonate group Chemical group 0.000 claims description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 3
- 235000019387 fatty acid methyl ester Nutrition 0.000 claims description 3
- 239000001397 quillaja saponaria molina bark Substances 0.000 claims description 3
- 229930182490 saponin Natural products 0.000 claims description 3
- 150000007949 saponins Chemical class 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 230000014759 maintenance of location Effects 0.000 abstract 1
- 230000000630 rising effect Effects 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 7
- 239000007788 liquid Substances 0.000 description 7
- 239000003784 tall oil Substances 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 238000001704 evaporation Methods 0.000 description 4
- 230000008020 evaporation Effects 0.000 description 4
- 239000002253 acid Substances 0.000 description 2
- 238000004537 pulping Methods 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerol Natural products OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 1
- 235000019687 Lamb Nutrition 0.000 description 1
- 235000008331 Pinus X rigitaeda Nutrition 0.000 description 1
- 235000011613 Pinus brutia Nutrition 0.000 description 1
- 241000018646 Pinus brutia Species 0.000 description 1
- 235000011609 Pinus massoniana Nutrition 0.000 description 1
- 241000018650 Pinus massoniana Species 0.000 description 1
- 229920001131 Pulp (paper) Polymers 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000007799 cork Substances 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 235000011187 glycerol Nutrition 0.000 description 1
- 150000002632 lipids Chemical class 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 159000000000 sodium salts Chemical group 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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- Extraction Or Liquid Replacement (AREA)
Abstract
Disclosed are saponifiable matter extraction method and a saponifiable matter extraction device. Saponifiable matters are allowed to stay in a black liquor tank and are extracted from black liquor by separating, and surfactant accounting for 0.2-0.5% of the black liquor by weight or sodium sulfonate accounting for 1%-2% of the black liquor by weight is added in the separating process. The saponifiable matter extraction device comprises the black liquor tank which is provided with at least two saponifiable matter outlets, one saponifiable matter outlet is located at the top of the black liquortank, other saponifiable matter outlets are lower than the first saponifiable matter outlet and provided with openable gates. The speed of separating and rising of the saponifiable matters can be increased, the time of retention and separation of the saponifiable matters can be adjusted according to production conditions, the saponifiable matters are recycled timely, and accordingly deteriorationof the saponifiable matters is prevented, and the extraction rate of the saponifiable matters is increased.
Description
Technical field
The present invention relates to the saponified recovery technology of pulping and papermaking processes field, especially relate to the saponified method of extraction from black liquor; The invention still further relates to the saponified a kind of device of extraction from black liquor.
Background technology
In cork alkaline process process, the resinous acid that disengages with various saponified sodium-salt forms, lipid acid and saponifiable matter not enter vapo(u)rization system after black liquid extraction, it has been reclaimed important economic value, it is fully reclaimed, also be conducive to the evaporation operation that alkali reclaims.
Traditional saponified extracting method, the rare black liquor of slurrying, leave standstill through half concentrated black liquid groove behind finite concentration through evaporation concentration, saponifiedly extract after standing separation at the black liquor groove.A kind of tall oil recovery method is disclosed as CN101392148A, be in the alkaline process paper process of raw material with the pine, paper pulp is isolated black liquor of pulp making through washing after the boiling, sending evaporation section to be concentrated into concentration through dehydration by evaporation black liquor is 35～45% half concentrated black liquid, after leaving standstill, the saponified storage tank top that floats in half concentrated black liquid is collected saponified from the top of half concentrated black liquid storage tank.
Because traditional saponified extracting method is subjected to the influence of saponified separator tank liquid level in the production process bigger, stop disengaging time and be difficult to the state that reaches desirable, the saponified speed of separating from black liquor is lower in addition, and saponified separating effect is undesirable, and saponified extraction yield is low.
Summary of the invention
In order to overcome the defective of prior art, on the one hand, one of technical problem to be solved by this invention provides a kind of separation efficiency height, saponified extracting method that extraction yield is high.
In order to solve the problems of the technologies described above, the invention provides a kind of saponified extracting method, its basic technical scheme is: extract saponified the separation from black liquor after stopping in the black liquor groove, adds the tensio-active agent of black liquor weight 0.2wt%～0.5wt% and/or the sodium sulfate of 1wt%～2wt% in sepn process.
Preferably, the saponified time that stops separation in the black liquor groove is 2.5～3.5 hours.
Preferably, the saponified solid concentration that stops black liquor when separating in the black liquor groove is 22%～30%.
Preferably, the saponified temperature that stops black liquor when separating in the black liquor groove is 70～90 ℃.
Further, the saponified stop in the black liquor groove when separating feeds pressurized air at described black liquor trench bottom and accelerates saponified separation.
Preferably, described tensio-active agent is one or more in Sodium dodecylbenzene sulfonate, fatty alcohol polyoxyethylene ether sulfate, secondary alkyl sulfonate, alpha-olefin sodium sulfonate, alpha-sulfo fatty acid methyl ester sodium, aliphatic alcohol polyethenoxy ether carboxylate, tea saponin, the polypeptide based surfactants.
On the other hand, one of technical problem to be solved by this invention provides a kind of can the flexible adaptation production process variation, make saponified separation be in the saponified extraction element of preferred process state.
In order to solve the problems of the technologies described above, the invention provides a kind of saponified extraction element, its basic technical scheme is: this device comprises the black liquor groove, described black liquor groove is provided with at least two saponified outlets, wherein the first saponified outlet is positioned at the top of described black liquor groove, and the installation site of all the other saponified outlets is lower than the described first saponified outlet and all the other saponified outlets are provided with the gate that can open or close.
Further, the black liquor trench bottom of saponified extraction element also has compressed air line and sparger.
Further, the black liquor groove inside of saponified extraction element is provided with the cofferdam identical with described saponified export volume, and described cofferdam is fixed on black liquor groove inwall, and the outlet of described cofferdam is connected with described saponified outlet.
The beneficial effect that the present invention brings: in saponified stop sepn process, add tensio-active agent, can accelerate saponified separation lift velocity; In saponified stop sepn process, add sodium sulfate, reduced saponified solubleness in black liquor, improve saponified extraction yield; Saponified extraction element is provided with at least two saponified outlets that the installation site height is different, can be according to the height of the liquid level in the saponified separation black liquor groove, open the saponified outlet of different heights flexibly, adjust saponified stop disengaging time according to the condition of production, in time reclaim saponified, prevent from causing saponified rottenly because of long time stored, improve saponified extraction yield.
Description of drawings
Below in conjunction with the drawings and specific embodiments content of the present invention is described in further detail:
Fig. 1 is the saponified extraction element master of embodiment of the invention TV structure synoptic diagram;
Fig. 2 is that A-A of Fig. 1 is to structural representation.
Embodiment
As Fig. 1, the saponified extraction element of embodiment shown in Figure 2, this device comprises black liquor groove 7, black liquor groove 7 is provided with two saponified outlets 1 and 3, wherein the first saponified outlet 1 is positioned at the top of black liquor groove 7, the installation site of another saponified outlet 3 is lower than the position of the first saponified outlet 1, and saponified outlet 3 is provided with the gate 4 that can open or close, black liquor groove 7 inside are provided with cofferdam 2 and 5, cofferdam 2 and 5 is fixed on black liquor groove inwall, the outlet in cofferdam 2 is connected with the first saponified outlet 1, the outlet in cofferdam 5 is connected with saponified outlet 3, and the bottom of black liquor groove 7 also has compressed air line 8 and sparger 6.
Embodiment 1: use aforementioned saponified extraction element to extract when saponified, the black liquor that the slurrying extraction obtains is concentrated to temperature in evaporative process be 75 ℃, black liquor solid concentration is 24% black liquor, be sent in the black liquor groove 7, in this black liquor, add black liquor amount 0.2wt% Sodium dodecylbenzene sulfonate tensio-active agent, also the bottom from compressed air line 8 and sparger 6 to black liquor groove 7 feeds pressurized air in stopping sepn process, accelerate saponified separation, this black liquor stops after 3.5 hours in black liquor groove 7, partly-hydrolysed thing is wherein analysed day, rise to the top of black liquor groove 7,2 from first saponified outlet 1 outflow through the cofferdam, thereby obtain saponified.
Embodiment 2: use aforementioned saponified extraction element to extract when saponified, the black liquor that the slurrying extraction obtains is concentrated to temperature in evaporative process be 85 ℃, black liquor solid concentration is 27% black liquor, be sent in the black liquor groove 7, the polypeptide based surfactants that in this black liquor, adds black liquor amount 0.5wt%, also the bottom from compressed air line 8 and sparger 6 to black liquor groove 7 feeds pressurized air in stopping sepn process, accelerate saponified separation, this black liquor stops after 2.5 hours in black liquor groove 7, partly-hydrolysed thing is wherein analysed day, rise to the top of black liquor groove 7,2 from first saponified outlet 1 outflow through the cofferdam, thereby obtain saponified.
Embodiment 3: use aforementioned saponified extraction element to extract when saponified, the black liquor that the slurrying extraction obtains is concentrated to temperature in evaporative process be 84 ℃, black liquor solid concentration is 27.5% black liquor, be sent in the black liquor groove 7, the alpha-olefin sodium sulfonate tensio-active agent that in this black liquor, adds black liquor amount 0.35wt%, also the bottom from compressed air line 8 and sparger 6 to black liquor groove 7 feeds pressurized air in stopping sepn process, accelerate saponified separation, this black liquor stops after 3 hours in black liquor groove 7, partly-hydrolysed thing is wherein analysed day, rise to the top of black liquor groove 7,2 from first saponified outlet 1 outflow through the cofferdam, thereby obtain saponified.
Embodiment 4: use aforementioned saponified extraction element to extract when saponified, the black liquor that the slurrying extraction obtains is concentrated to temperature in evaporative process be 70 ℃, black liquor solid concentration is 22% black liquor, be sent in the black liquor groove 7, the sodium sulfate that in this black liquor, adds black liquor amount 0.2wt% fatty alcohol polyoxyethylene ether sulfate tensio-active agent and 1wt%, this black liquor stops after 3.2 hours in black liquor groove 7, partly-hydrolysed thing is wherein analysed day, rise to the top of black liquor groove 7,5 from saponified outlet 3 outflows through the cofferdam, thereby obtain saponified.
Embodiment 5: use aforementioned saponified extraction element to extract when saponified, the black liquor that the slurrying extraction obtains is concentrated to temperature in evaporative process be 80 ℃, black liquor solid concentration is 26% black liquor, be sent in the black liquor groove 7, add the sodium sulfate of black liquor amount 2wt% in this black liquor, this black liquor stops after 3.5 hours in black liquor groove 7, partly-hydrolysed thing is wherein analysed day, rise to the top of black liquor groove 7,2 from first saponified outlet 1 outflow through the cofferdam, thereby obtain saponified.
Embodiment 6: use aforementioned saponified extraction element to extract when saponified, the black liquor that the slurrying extraction obtains is concentrated to temperature in evaporative process be 90 ℃, black liquor solid concentration is 30% black liquor, be sent in the black liquor groove 7, the sodium sulfate that in this black liquor, adds black liquor amount 1.5wt%, also the bottom from compressed air line 8 and sparger 6 to black liquor groove 7 feeds pressurized air in stopping sepn process, accelerate saponified separation, this black liquor stops after 2.6 hours in black liquor groove 7, partly-hydrolysed thing is wherein analysed day, rise to the top of black liquor groove 7,5 from saponified outlet 3 outflows through the cofferdam, thereby obtain saponified.
Comparative Examples 7: use aforementioned saponified extraction element to extract when saponified, the black liquor that the slurrying extraction obtains is concentrated to temperature in evaporative process be 65 ℃, black liquor solid concentration is 20% black liquor, be sent in the black liquor groove 7, stop after 2.2 hours in black liquor groove 7, partly-hydrolysed thing is wherein analysed day, rises to the top of black liquor groove 7,2 from first saponified outlet 1 outflow through the cofferdam, thereby obtain saponified.
Comparative Examples 8: use aforementioned saponified extraction element to extract when saponified, the black liquor that the slurrying extraction obtains is concentrated to temperature in evaporative process be 95 ℃, black liquor solid concentration is 32% black liquor, be sent in the black liquor groove 7, stop after 4 hours in black liquor groove 7, partly-hydrolysed thing is wherein analysed day, rises to the top of black liquor groove 7,2 from first saponified outlet 1 outflow through the cofferdam, thereby obtain saponified.
Comparative Examples 9: use aforementioned saponified extraction element to extract when saponified, the black liquor that the slurrying extraction obtains is concentrated to temperature in evaporative process be 68 ℃, black liquor solid concentration is 35% black liquor, be sent in the black liquor groove 7, stop after 5 hours in black liquor groove 7, partly-hydrolysed thing is wherein analysed day, rises to the top of black liquor groove 7,2 from first saponified outlet 1 outflow through the cofferdam, thereby obtain saponified.
Through to above embodiment or Comparative Examples test, when producing the Pinus massoniana Lamb sulfate pulping, Tall oil quantity such as following table that the ton slurry reclaims from saponified:
| Embodiment | Embodiment 1 | Embodiment 2 | Embodiment 3 | |
|
Embodiment 6 | Comparative Examples 7 | Comparative Examples 8 | Comparative Examples 9 |
| Ton slurry Tall oil reclaims quantity kg | 31.21 | 32.07 | 32.41 | 30.02 | 31.76 | 31.23 | 19.13 | 26.32 | 25.18 |
Test result shows that also the saponified solid concentration that stops black liquor when separating in the black liquor groove is, can reclaim more Tall oil at 22%～30% o'clock, and concentration reduces or raises, and the yield of Tall oil will reduce; When not adding tensio-active agent or using pressurized air, the saponified time that stops separation in the black liquor groove still can not fully separate when reaching 3.5 hours, if it is fully separated, black liquor need have less liquid-column height when stopping, add tensio-active agent or use pressurized air to be conducive to accelerate saponified separation; Add sodium sulfate and be conducive to improve saponified yield rate.
The tensio-active agent that adds can be in Sodium dodecylbenzene sulfonate, fatty alcohol polyoxyethylene ether sulfate, secondary alkyl sulfonate, alpha-olefin sodium sulfonate, alpha-sulfo fatty acid methyl ester sodium, aliphatic alcohol polyethenoxy ether carboxylate, tea saponin, the polypeptide based surfactants one or more.Can also be quaternized thing, glycerin fatty acid ester etc.
The above is the preferred embodiments of the present invention only, and does not limit the present invention in any way, and for a person skilled in the art, the present invention can have various changes and variation.Within the spirit and principles in the present invention all, any modification of doing, be equal to replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (5)
1. saponified extracting method, is characterized in that: add the tensio-active agent of black liquor weight 0.2wt%～0.5wt% and/or the sodium sulfate of 1wt%～2wt% in sepn process saponified separation from black liquor after stopping in the black liquor groove and extracting; Described black liquor groove is provided with at least two saponified outlets, wherein the first saponified outlet is positioned at the top of described black liquor groove, and the installation site of all the other saponified outlets is lower than the described first saponified outlet and all the other saponified outlets are provided with the gate that can open or close; Described black liquor groove inside is provided with the cofferdam identical with described saponified export volume, and described cofferdam is fixed on black liquor groove inwall, and the outlet of described cofferdam is connected with described saponified outlet
The described saponified time that stops separation in the black liquor groove is 2.5～3.5 hours.
2. saponified extracting method according to claim 1 is characterized in that: the described saponified solid concentration that stops black liquor when separating in the black liquor groove is 22%～30%.
3. saponified extracting method according to claim 1 is characterized in that: the described saponified temperature that stops black liquor when separating in the black liquor groove is 70～90 ℃.
4. saponified extracting method according to claim 1, it is characterized in that: described black liquor trench bottom also has compressed air line and sparger; Described saponified the stop in the black liquor groove when separating feeds pressurized air at described black liquor trench bottom and accelerates saponified separation.
5. saponified extracting method according to claim 1, it is characterized in that: described tensio-active agent is one or more in Sodium dodecylbenzene sulfonate, fatty alcohol polyoxyethylene ether sulfate, secondary alkyl sulfonate, alpha-olefin sodium sulfonate, alpha-sulfo fatty acid methyl ester sodium, aliphatic alcohol polyethenoxy ether carboxylate, tea saponin, the polypeptide based surfactants.
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| CN 201210122344 CN102643612B (en) | 2012-04-25 | 2012-04-25 | Saponifiable matter extraction method and saponifiable matter extraction device |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102852021A (en) * | 2012-09-11 | 2013-01-02 | 长沙理工大学 | Black liquor tank used in saponification product extraction, and saponification product extraction method |
| CN103357194B (en) * | 2013-06-14 | 2016-02-17 | 武汉轻工大学 | The extractant of synchronous production cape jasmine multiple efficacies component and Extraction and isolation method thereof |
| CN106049151B (en) * | 2016-08-22 | 2018-03-20 | 湖南双阳高科化工有限公司 | A kind of device and method from saponified middle separation black liquor |
Citations (3)
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|---|---|---|---|---|
| US4879369A (en) * | 1988-01-20 | 1989-11-07 | Westvaco Corporation | Method of removing lignin from tall oil |
| CN1668805A (en) * | 2002-07-23 | 2005-09-14 | 纳尔科公司 | Process for deresinizing pulp using alkoxylated alkyl alcohol surfactants |
| JP2010516872A (en) * | 2007-01-26 | 2010-05-20 | ナルコ カンパニー | Additives to increase the separation yield of tall oil soap from black liquor |
-
2012
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4879369A (en) * | 1988-01-20 | 1989-11-07 | Westvaco Corporation | Method of removing lignin from tall oil |
| CN1668805A (en) * | 2002-07-23 | 2005-09-14 | 纳尔科公司 | Process for deresinizing pulp using alkoxylated alkyl alcohol surfactants |
| JP2010516872A (en) * | 2007-01-26 | 2010-05-20 | ナルコ カンパニー | Additives to increase the separation yield of tall oil soap from black liquor |
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| Title |
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| 《造纸工业碱回收》编写组.《造纸工业碱回收》.《造纸工业碱回收》.轻工业出版社,1977,(第1版),第71-72页. * |
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Address after: 418005 Huaihua Industrial Park, Hunan, Huaihua Patentee after: Hunan Jun Thai New Materials Technology Co. Ltd. Address before: 418005 Huaihua Industrial Park, Hunan, Huaihua Patentee before: Hu'nan Juntai Pulp Paper Co., Ltd. |