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CN111974018B - A kind of efficient condensation collection and separation method of biomass pyrolysis gas - Google Patents

A kind of efficient condensation collection and separation method of biomass pyrolysis gas Download PDF

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CN111974018B
CN111974018B CN202010910891.XA CN202010910891A CN111974018B CN 111974018 B CN111974018 B CN 111974018B CN 202010910891 A CN202010910891 A CN 202010910891A CN 111974018 B CN111974018 B CN 111974018B
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王傲
龚建平
卢辛成
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D5/00Condensation of vapours; Recovering volatile solvents by condensation
    • B01D5/0078Condensation of vapours; Recovering volatile solvents by condensation characterised by auxiliary systems or arrangements
    • B01D5/009Collecting, removing and/or treatment of the condensate
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D3/00Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/14Fractional distillation or use of a fractionation or rectification column
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D5/00Condensation of vapours; Recovering volatile solvents by condensation
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    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10BDESTRUCTIVE DISTILLATION OF CARBONACEOUS MATERIALS FOR PRODUCTION OF GAS, COKE, TAR, OR SIMILAR MATERIALS
    • C10B53/00Destructive distillation, specially adapted for particular solid raw materials or solid raw materials in special form
    • C10B53/02Destructive distillation, specially adapted for particular solid raw materials or solid raw materials in special form of cellulose-containing material
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    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10CWORKING-UP PITCH, ASPHALT, BITUMEN, TAR; PYROLIGNEOUS ACID
    • C10C5/00Production of pyroligneous acid distillation of wood, dry distillation of organic waste
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Abstract

本发明公开了一种生物质热解气体高效冷凝收集分离方法,属于可再生能源利用技术领域。采用生物质热解气体高效冷凝收集分离装置,生物质热解气体经过管式冷凝装置进行充分冷凝;冷凝得到的液体转移至收集罐中进行静置分层,取上层清液即为粗木醋液;粗木醋液加入分离提纯装置中,对粗木醋液进行分离提纯,得到精制木醋液。本发明以不同尺寸玻璃珠为精馏装置填充物,通过调控不同尺寸玻璃珠的体积比就可实现不同类型木醋液的定向提纯与分离,可以获得多种类高品质的木醋液,方法简单,易推广。

Figure 202010910891

The invention discloses a method for efficiently condensing, collecting and separating biomass pyrolysis gas, which belongs to the technical field of renewable energy utilization. The biomass pyrolysis gas high-efficiency condensation collection and separation device is adopted, and the biomass pyrolysis gas is fully condensed through the tubular condensation device; the liquid obtained by condensation is transferred to the collection tank for standing and stratification, and the supernatant liquid is taken as crude wood vinegar The crude wood vinegar is added to the separation and purification device, and the crude wood vinegar is separated and purified to obtain a refined wood vinegar. In the invention, glass beads of different sizes are used as fillers in the rectification device, and the directional purification and separation of different types of wood vinegar can be realized by adjusting the volume ratio of glass beads of different sizes, and various types of high-quality wood vinegar can be obtained, and the method is simple , easy to promote.

Figure 202010910891

Description

一种生物质热解气体高效冷凝收集分离方法A kind of efficient condensation collection and separation method of biomass pyrolysis gas

技术领域technical field

本发明属于可再生能源利用技术领域,具体涉及一种生物质热解气体高效冷凝收集分离方法。The invention belongs to the technical field of renewable energy utilization, and in particular relates to a method for efficient condensation, collection and separation of biomass pyrolysis gas.

背景技术Background technique

生物质热解制备生物炭是废弃生物质或加工剩余物高值化应用的一种重要方式,具有显著的经济、社会和生态效益。然而,除炭之外,热解过程还会产生很多气体,这些热解气体中富含焦油、醋液等有机物和大量的水,如果不能有效冷凝收集和分离将会导致环境污染和资源浪费。尤其是冷凝得到的木醋液,因为含有多种有机物,包括有机酸、酚和醛等,可以作为有机肥添加剂、畜禽饲料、防腐剂、燃料、保健药,具有极高的应用价值。然而,目前的生物质热解气冷凝、收集和分离工艺十分落后,尤其是木醋液的高效分离提纯技术缺乏,导致热解气难以充分和高值利用。Biomass pyrolysis to prepare biochar is an important way for high-value application of waste biomass or processing residues, and has significant economic, social and ecological benefits. However, in addition to carbon, the pyrolysis process will also produce a lot of gases. These pyrolysis gases are rich in tar, vinegar and other organic substances and a large amount of water. If they cannot be effectively condensed, collected and separated, it will lead to environmental pollution and waste of resources. Especially the wood vinegar obtained by condensation, because it contains a variety of organic substances, including organic acids, phenols and aldehydes, etc., can be used as organic fertilizer additives, livestock and poultry feeds, preservatives, fuels, health care drugs, and has extremely high application value. However, the current biomass pyrolysis gas condensation, collection and separation technology is very backward, especially the lack of efficient separation and purification technology of wood vinegar, resulting in the difficulty of fully and high-value utilization of pyrolysis gas.

发明内容SUMMARY OF THE INVENTION

针对现有技术中存在的问题,本发明要解决的技术问题在于提供了一种生物质热解气体高效冷凝收集分离技术工艺,可以实现木醋液的定向高效冷凝、提纯。Aiming at the problems existing in the prior art, the technical problem to be solved by the present invention is to provide a high-efficiency condensation collection and separation technology process of biomass pyrolysis gas, which can realize the directional high-efficiency condensation and purification of wood vinegar.

为了解决上述问题,本发明所采用的技术方案如下:In order to solve the above problems, the technical scheme adopted in the present invention is as follows:

一种生物质热解气体高效冷凝收集分离方法,包括以下步骤:A method for efficient condensation, collection and separation of biomass pyrolysis gas, comprising the following steps:

(1)采用生物质热解气体高效冷凝收集分离装置,生物质热解气体经过管式冷凝装置进行充分冷凝;(1) Adopt biomass pyrolysis gas high-efficiency condensation collection and separation device, biomass pyrolysis gas is fully condensed through tubular condensation device;

(2)冷凝得到的液体转移至收集罐中进行静置分层,取上层清液即为粗木醋液;(2) the liquid obtained by condensation is transferred to the collecting tank to carry out stratification by standing, and getting the supernatant liquid is thick wood vinegar;

(3)粗木醋液加入分离提纯装置,对粗木醋液进行分离提纯,得到精制木醋液。(3) The crude wood vinegar is added to a separation and purification device, and the crude wood vinegar is separated and purified to obtain a refined wood vinegar.

所述生物质热解气体高效冷凝收集分离方法,所述管式冷凝装置为U型,其中填充物有铁丝网或玻璃纤维,填充量为管式冷凝装置体积的80%~90%。In the method for efficient condensation, collection and separation of biomass pyrolysis gas, the tubular condensing device is U-shaped and filled with barbed wire or glass fiber, and the filling amount is 80% to 90% of the volume of the tubular condensing device.

所述生物质热解气体高效冷凝收集分离方法,所述的分离提纯装置中精馏温度为100~120℃。In the method for efficient condensation, collection and separation of biomass pyrolysis gas, the rectification temperature in the separation and purification device is 100-120°C.

所述生物质热解气体高效冷凝收集分离方法,所述的分离提纯装置中填充物为的玻璃珠;玻璃珠的填充高度为分馏柱高度的4/5。In the method for efficient condensation, collection and separation of biomass pyrolysis gas, the filler in the separation and purification device is glass beads; the filling height of the glass beads is 4/5 of the height of the fractionation column.

所述生物质热解气体高效冷凝收集分离方法,所述的分离提纯过程中重组分与轻组分的回流比为4:1~3:2。In the method for efficient condensation, collection and separation of biomass pyrolysis gas, the reflux ratio of heavy components to light components in the separation and purification process is 4:1 to 3:2.

所述生物质热解气体高效冷凝收集分离方法,所述玻璃珠的直径有5mm、3mm和1mm,三种尺寸玻璃珠的装填体积比为4:2:1。In the method for efficient condensation collection and separation of biomass pyrolysis gas, the diameters of the glass beads are 5 mm, 3 mm and 1 mm, and the packing volume ratio of the three sizes of glass beads is 4:2:1.

所述生物质热解气体高效冷凝收集分离方法,分馏柱从下到下按照不同尺寸玻璃珠的装填体积分别填充5mm玻璃珠、3mm玻璃珠、1mm玻璃珠。In the method for efficient condensation, collection and separation of biomass pyrolysis gas, the fractionation column is filled with 5mm glass beads, 3mm glass beads, and 1mm glass beads according to the filling volume of glass beads of different sizes from bottom to bottom.

所述生物质热解气体高效冷凝收集分离方法,生物质热解气体高效冷凝收集分离装置包括冷凝段、收集段和分离提纯段;所述冷凝段包括一个U型的管式冷凝装置,所述管式冷凝装置上设有热解气体进口;所述收集段包括一个收集罐;In the method for efficient condensation collection and separation of biomass pyrolysis gas, the biomass pyrolysis gas efficient condensation collection and separation device includes a condensation section, a collection section and a separation and purification section; the condensation section includes a U-shaped tubular condensation device, and the The tubular condensing device is provided with a pyrolysis gas inlet; the collection section includes a collection tank;

所述分离提纯段包括分离提纯装置、分馏柱、产物收集罐、产物气体管道、冷凝水回流管道和冷凝水进水口,所述分离提纯装置上方设有分馏柱,所述分馏柱的上部设有温度计和产物气体管道,产物气体管道的另一端与产物收集罐连接,所述产物气体管道外面设有冷凝水管道,所述冷凝水管道上设有冷凝水进水口,冷凝水回流管道的两端与冷凝水管道和冷凝水进水口连通,形成冷凝水的回水通路。The separation and purification section includes a separation and purification device, a fractionation column, a product collection tank, a product gas pipeline, a condensed water return pipeline and a condensed water inlet. The separation and purification device is provided with a fractionation column, and the upper part of the fractionation column is provided with A thermometer and a product gas pipeline, the other end of the product gas pipeline is connected to a product collection tank, a condensed water pipeline is provided outside the product gas pipeline, a condensed water inlet is provided on the condensed water pipeline, and both ends of the condensed water return pipeline It is connected with the condensed water pipeline and the condensed water inlet to form the return water passage of the condensed water.

所述生物质热解气体高效冷凝收集分离方法,所述产物气体管道为夹角大于90°的弯管。In the method for efficient condensation, collection and separation of biomass pyrolysis gas, the product gas pipeline is an elbow with an included angle greater than 90°.

有益效果:与现有的技术相比,本发明的优点包括:Beneficial effects: Compared with the existing technology, the advantages of the present invention include:

(1)本发明以廉价的铁丝网或玻璃纤维为U型的管式冷凝装置的填充物,可以增加换热面积,提高换热效率,实现高效冷凝。(1) The present invention uses cheap wire mesh or glass fiber as the filler of the U-shaped tubular condensing device, which can increase the heat exchange area, improve the heat exchange efficiency, and realize efficient condensation.

(2)本发明分离提纯装置中的填充物为玻璃珠,廉价易得,通过调控不同尺寸玻璃珠的体积比就可实现不同类型木醋液的定向提纯与分离,获得多种类高品质的木醋液,实现热解气体的高效冷凝收集和分离;方法简单,易推广。(2) The filler in the separation and purification device of the present invention is glass beads, which are cheap and easy to obtain. By adjusting the volume ratio of glass beads of different sizes, the directional purification and separation of different types of wood vinegar can be realized, and various types of high-quality wood vinegar can be obtained. Vinegar liquid can realize efficient condensation collection and separation of pyrolysis gas; the method is simple and easy to popularize.

附图说明Description of drawings

图1为生物质热解气体高效冷凝收集分离装置结构示意图。FIG. 1 is a schematic structural diagram of a high-efficiency condensation, collection and separation device for biomass pyrolysis gas.

具体实施方式Detailed ways

为使本发明的上述目的、特征和优点能够更加明显易懂,下面结合具体实施例对本发明的具体实施方式做详细的说明。In order to make the above objects, features and advantages of the present invention more clearly understood, the specific embodiments of the present invention will be described in detail below with reference to specific embodiments.

生物质热解气体高效冷凝收集分离装置包括冷凝段、收集段和分离提纯段;冷凝段包括一个U型的管式冷凝装置2,管式冷凝装置2上设有热解气体进口1;收集段包括收集罐3;The biomass pyrolysis gas high-efficiency condensation collection and separation device includes a condensation section, a collection section and a separation and purification section; the condensation section includes a U-shaped tubular condensation device 2, and the tubular condensation device 2 is provided with a pyrolysis gas inlet 1; The collection section Including collection tank 3;

分离提纯段包括分离提纯装置4、分馏柱5、产物收集罐7、产物气体管道8、冷凝水回流管道9和冷凝水进水口10,分离提纯装置4上方设有分馏柱5,分馏柱5的上部设有温度计6和产物气体管道8,产物气体管道8为夹角大于90°的弯管,产物气体管道8的设计使其分为两端,靠近分馏柱5的一段,在冷凝水的作用下,一部分气体冷凝之后再次进入分馏柱开始蒸馏过程,相当于对物质进行了又一次的分离提纯,提高分离提纯效果;The separation and purification section includes a separation and purification device 4, a fractionation column 5, a product collection tank 7, a product gas pipeline 8, a condensed water reflux pipeline 9 and a condensed water inlet 10. The separation and purification device 4 is provided with a fractionation column 5 above. The upper part is provided with a thermometer 6 and a product gas pipeline 8, the product gas pipeline 8 is an elbow with an included angle greater than 90°, and the product gas pipeline 8 is designed to be divided into two ends, close to a section of the fractionation column 5, in the role of the condensed water. After the condensation, a part of the gas enters the fractionation column again to start the distillation process, which is equivalent to performing another separation and purification on the substance to improve the separation and purification effect;

产物气体管道8的另一端与产物收集罐7连接,产物气体管道8外面设有冷凝水管道,冷凝水管道上设有冷凝水进水口10,冷凝水回流管道9的两端与冷凝水管道和冷凝水进水口10连通,形成冷凝水的回水通路。下面实施例1~3均采用该装置进行杉木屑热解气体的高效冷凝收集分离过程。The other end of the product gas pipeline 8 is connected with the product collection tank 7, the product gas pipeline 8 is provided with a condensed water pipeline, the condensed water pipeline is provided with a condensed water inlet 10, and the two ends of the condensed water return pipeline 9 are connected with the condensed water pipeline and The condensed water inlet 10 is connected to form a return water passage of the condensed water. The following embodiments 1 to 3 all use this device to carry out the high-efficiency condensation collection and separation process of the pyrolysis gas of Chinese fir chips.

实施例1Example 1

一种生物质热解气体高效冷凝收集分离方法,包括以下步骤:A method for efficient condensation, collection and separation of biomass pyrolysis gas, comprising the following steps:

(1)氮气吹扫下,杉木屑100g在450℃条件下热解0.5h,收集热解气体;(1) Under nitrogen purging, 100g of Chinese fir chips were pyrolyzed at 450°C for 0.5h, and the pyrolysis gas was collected;

(2)将热解气体通入装填有铁丝网的U型的管式冷凝装置2中,收集所得冷凝液体转移至收集罐3中;(2) the pyrolysis gas is passed into the U-shaped tubular condensing device 2 filled with wire mesh, and the collected condensed liquid is transferred to the collection tank 3;

(3)将冷凝液体静置1天后,分层,上层清液转移至分离提纯装置,开始分离提纯;(3) after the condensed liquid is left standstill for 1 day, the layers are separated, and the supernatant liquid is transferred to the separation and purification device, and the separation and purification is started;

(4)控制精馏温度为105℃,分馏柱5长45cm,直径10cm,填充玻璃球高度36cm,5mm玻璃球:3mm玻璃球:1mm玻璃球的体积比为4:2:1,回流比为4:1,收集下层重相木醋液。(4) Control the rectification temperature to be 105°C, the fractionation column 5 is 45cm long, 10cm in diameter, the height of the filled glass balls is 36cm, the volume ratio of 5mm glass balls: 3mm glass balls: 1mm glass balls is 4:2:1, and the reflux ratio is 4:1, collect the lower heavy phase wood vinegar.

实施例2Example 2

一种生物质热解气体高效冷凝收集分离方法,包括以下步骤:A method for efficient condensation, collection and separation of biomass pyrolysis gas, comprising the following steps:

(1)氮气吹扫下,杉木屑100g在450℃条件下热解0.5h,收集热解气体;(1) Under nitrogen purging, 100g of Chinese fir chips were pyrolyzed at 450°C for 0.5h, and the pyrolysis gas was collected;

(2)将热解气体通入装填有铁丝网的U型的管式冷凝装置2中,收集所得冷凝液体转移至收集罐3中;(2) the pyrolysis gas is passed into the U-shaped tubular condensing device 2 filled with wire mesh, and the collected condensed liquid is transferred to the collection tank 3;

(3)将冷凝液体静置1天后,分层,将上层清液转移至分离提纯装置,开始分离提纯;(3) after the condensed liquid is left standstill for 1 day, the layers are separated, and the supernatant liquid is transferred to the separation and purification device, and the separation and purification is started;

(4)控制精馏温度为110℃,分馏柱5长45cm,直径10cm,填充玻璃球高度36cm,5mm玻璃球:3mm玻璃球:1mm玻璃球的体积比为2:1:1,回流比为4:1,收集下层重相木醋液。(4) Control the rectification temperature to be 110°C, the fractionation column 5 is 45cm long, 10cm in diameter, the height of the filled glass balls is 36cm, the volume ratio of 5mm glass balls: 3mm glass balls: 1mm glass balls is 2:1:1, and the reflux ratio is 4:1, collect the lower heavy phase wood vinegar.

实施例3Example 3

一种生物质热解气体高效冷凝收集分离方法,包括以下步骤:A method for efficient condensation, collection and separation of biomass pyrolysis gas, comprising the following steps:

(1)氮气吹扫下,杉木屑100g在450℃条件下热解0.5h,收集热解气体;(1) Under nitrogen purging, 100g of Chinese fir chips were pyrolyzed at 450°C for 0.5h, and the pyrolysis gas was collected;

(2)将热解气体通入装填有铁丝网的U型的管式冷凝装置2中,收集所得冷凝液体转移至收集罐3中;(2) the pyrolysis gas is passed into the U-shaped tubular condensing device 2 filled with wire mesh, and the collected condensed liquid is transferred to the collection tank 3;

(3)将冷凝液体静置1天后,分层,将上层清液转移至分离提纯装置,开始分离提纯;(3) after the condensed liquid is left standstill for 1 day, the layers are separated, and the supernatant liquid is transferred to the separation and purification device, and the separation and purification is started;

(4)控制精馏温度为105℃,分馏柱5长45cm,直径10cm,填充玻璃球高度36cm,5mm玻璃球:3mm玻璃球:1mm玻璃球的体积比为4:2:1,回流比为3:2,收集下层重相木醋液。(4) Control the rectification temperature to be 105°C, the fractionation column 5 is 45cm long, 10cm in diameter, the height of the filled glass balls is 36cm, the volume ratio of 5mm glass balls: 3mm glass balls: 1mm glass balls is 4:2:1, and the reflux ratio is 3:2, collect the lower heavy phase wood vinegar.

对实施例1~3收集的重相木醋液的有机组分及pH进行测定,结果如表1所示。由表1可知,本发明很高效的实现了杉木屑热解气体的冷凝收集分离。The organic components and pH of the heavy-phase wood vinegar collected in Examples 1-3 were measured, and the results are shown in Table 1. It can be seen from Table 1 that the present invention effectively realizes the condensation, collection and separation of the pyrolysis gas of Chinese fir chips.

表1实施例1~3中精制木醋液有机组分含量及pH值结果Table 1 embodiment 1~3 in the refined wood vinegar organic component content and pH value result

实施例Example pHpH 有机酸含量(%)Organic acid content (%) 酚含量(%)Phenol content (%) 11 2.52.5 8.58.5 0.60.6 22 2.02.0 10.010.0 1.01.0 33 3.13.1 6.56.5 0.30.3

Claims (1)

1. A method for efficiently condensing, collecting and separating biomass pyrolysis gas is characterized by comprising the following steps:
(1) a biomass pyrolysis gas efficient condensation, collection and separation device is adopted, and the biomass pyrolysis gas is fully condensed through a tubular condensation device;
the high-efficiency condensation, collection and separation device for the biomass pyrolysis gas comprises a condensation section, a collection section and a separation and purification section; the condensation section comprises a U-shaped tubular condensation device (2), wherein the filler is an iron wire net or glass fiber, and the filling amount is 80-90% of the volume of the tubular condensation device; a pyrolysis gas inlet (1) is formed in the tubular condensing device (2); the collecting section comprises a collecting tank (3);
the separation and purification section comprises a separation and purification device (4), a fractionating column (5), a product collecting tank (7), a product gas pipeline (8), a condensed water backflow pipeline (9) and a condensed water inlet (10), the fractionating column (5) is arranged above the separation and purification device (4), a thermometer (6) and a product gas pipeline (8) are arranged at the upper part of the fractionating column (5), the product gas pipeline (8) is a bent pipe with an included angle larger than 90 degrees, the product gas pipeline (8) is divided into two ends and is close to one section of the fractionating column (5), and under the action of condensed water, part of gas is condensed and then enters the fractionating column again to start a distillation process; the other end of the product gas pipeline (8) is connected with the product collecting tank (7), a condensed water pipeline is arranged outside the product gas pipeline (8), a condensed water inlet (10) is formed in the condensed water pipeline, and two ends of a condensed water backflow pipeline (9) are communicated with the condensed water pipeline and the condensed water inlet (10) to form a condensed water return passage; the rectification temperature in the separation and purification device is 100-120 ℃; the filler is glass beads, the separation column is filled with glass beads with the diameters of 5mm, 3mm and 1mm respectively from bottom to top according to the filling volumes of the glass beads with different sizes, and the filling volume ratio of the glass beads with the three sizes is 4:2: 1; the packing height of the glass beads is 4/5 of the height of the fractionating column; the reflux ratio of the heavy component to the light component in the separation and purification process is 4: 1-3: 2;
(2) transferring the liquid obtained by condensation to a collection tank for standing and layering, and taking supernatant as crude pyroligneous liquor;
(3) adding the crude pyroligneous liquor into a separation and purification device, and separating and purifying the crude pyroligneous liquor to obtain refined pyroligneous liquor.
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