NL2035788B1 - Modified hydroxylpropyl starch and preparation method therefor and application thereof - Google Patents
Modified hydroxylpropyl starch and preparation method therefor and application thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B31/00—Preparation of derivatives of starch
- C08B31/08—Ethers
- C08B31/12—Ethers having alkyl or cycloalkyl radicals substituted by heteroatoms, e.g. hydroxyalkyl or carboxyalkyl starch
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
- C04B28/02—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing hydraulic cements other than calcium sulfates
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
- C04B28/02—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing hydraulic cements other than calcium sulfates
- C04B28/021—Ash cements, e.g. fly ash cements ; Cements based on incineration residues, e.g. alkali-activated slags from waste incineration ; Kiln dust cements
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
- C04B28/14—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing calcium sulfate cements
- C04B28/142—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing calcium sulfate cements containing synthetic or waste calcium sulfate cements
- C04B28/144—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing calcium sulfate cements containing synthetic or waste calcium sulfate cements the synthetic calcium sulfate being a flue gas desulfurization product
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L3/00—Compositions of starch, amylose or amylopectin or of their derivatives or degradation products
- C08L3/04—Starch derivatives, e.g. crosslinked derivatives
- C08L3/08—Ethers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L1/00—Compositions of cellulose, modified cellulose or cellulose derivatives
- C08L1/08—Cellulose derivatives
- C08L1/26—Cellulose ethers
- C08L1/28—Alkyl ethers
- C08L1/284—Alkyl ethers with hydroxylated hydrocarbon radicals
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Structural Engineering (AREA)
- Medicinal Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Polymers & Plastics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Biochemistry (AREA)
- Combustion & Propulsion (AREA)
- Curing Cements, Concrete, And Artificial Stone (AREA)
- Sealing Material Composition (AREA)
Abstract
Disclosed are modified hydroxypropyl starch and a preparation method therefor and an application thereof, relating to the technical field of building additives. The modified hydroxypropyl starch is prepared from the following raw materials in percent by mass: 5 - 40% of hydroxypropyl starch, 48 - 93% of cellulose ether, 1.5 - 8% of a dispersion enhancer, and 0.5 - 4% of a rheological stabilizer. The hydroxypropyl starch is prepared from the following raw materials in parts by mass: 0.8 - 1.2 parts of starch, 0.05 - 0.2 part of an inhibitor, 0.01 - 0.5 part of an alkalizer, 0.3 - 1 part of an alcohol, 10 0.05 - 0.3 part of an etherifying agent, and 0.0003 - 0.001 part of a crosslinking agent. The modified hydroxypropyl starch can be used in various building materials, and show excellent strength and Viscosity in putty, gypsum plaster, glue for tiles, and thermal mortar.
Description
MODIFIED HYDROXYLPROPYL STARCH AND PREPARATION METHOD
THEREFOR AND APPLICATION THEREOF
[01] The present invention relates to the technical field of building additives, and particularly relates to modified hydroxypropyl starch and a preparation method therefor and an application thereof.
[02] Hydroxypropyl starch rapidly improved in yield, usage amount and quality in recent years is widely applied to the industries of buildings, medicine, food, textile, papermaking, daily use chemicals, petroleum, and the like. Hydroxypropyl starch can also serve as an additive for cement-based products, gypsum-based products, and ash calcium products in the building field, is well compatible with other buildings and additives, and is particularly suitable for building dry blends such as mortar, binders, plastering materials, and roll plastering materials.
[03] A Chinese patent CN110590966B discloses a method for preparing modified hydroxypropyl starch capable of improving sliding performance of glue for tiles. The product is only applied to the anti-sliding aspect in the field of glue for tiles, and the performance only meets the requirements of CIT glue for tiles in the standard JC/T 547-2017. A Chinese patent CN113150176B introduces a method for preparing multi- group crosslinking modified hydroxypropyl cellulose ether. Although the product is subjected to crosslinking treatment with epoxy chloropropane, the product is only applied to the field of glue for tiles, and the performance only meets the requirements of
CIT glue for tiles in the standard JC/T 547-2017 as well. A Chinese patent
CN113444185A discloses high-viscosity hydroxypropyl cellulose ether and a preparation method therefor. The product is also subjected to crosslinking treatment with glyoxal, a specific viscosity index of the product is not specified, and specific application fields of the product are not specified as well.
[04] In conclusion, the strength and viscosity of hydroxypropyl starch in the prior art are limited, which hinders multi-purpose applications thereof in building materials.
[05] To make up for the deficiencies in the prior art, the present invention provides modified hydroxypropyl starch and a preparation method therefor and an application thereof. The modified hydroxypropyl starch provided by the present invention features high strength and viscosity.
[06] To achieve the above objective, the present invention provides the following technical solution:
[07] Modified hydroxypropyl starch, prepared from the following raw materials in percentage by mass: 5 - 40% of hydroxypropyl starch, 48 - 93% of cellulose ether, 1.5 - 8% of a dispersion enhancer, and 0.5 - 4% of a rheological stabilizer, where
[08] the hydroxypropyl starch is prepared from the following raw materials in parts by mass: 0.8 - 1.2 parts of starch, 0.05 - 0.2 part of an inhibitor, 0.01 - 0.5 part of an alkalizer, 0.3 - 1 part of alcohol, 0.05 - 0.3 part of an etherifying agent, and 0.0003 - 0.001 part of a crosslinking agent.
[09] Preferably, the cellulose ether is one or more of monobasic cellulose ether, binary cellulose ether, and ternary cellulose ether.
[10] Preferably, the dispersion enhancer is one or more of polyoxyethylene, sodium polyacrylate, polyacrylamide, polyvinyl alcohol, sodium alginate, and polycarboxylic acid.
[11] Preferably, the rheological stabilizer is one or more of guar gum, carrageenan,
Arabic gum, sesbania gum, flaxseed gum, and xanthan gum.
[12] Preferably, the inhibitor is sodium sulfate and/or potassium sulfate;
[13] the alkalizer is sodium hydroxide;
[14] the alcohol is ethanol;
[15] the etherifying agent is epoxypropane and/or sodium chloroacetate; and
[16] the crosslinking agent is epoxy chloropropane.
[17] The present invention further provides a method for preparing modified hydroxypropyl starch, including the following steps:
[18] alkalizing starch, an inhibitor, an alkalizer, an alcohol, an etherifying agent, and a crosslinking agent to obtain an alkalide;
[19] performing an etherification crosslinking reaction on the alkalide to obtain hydroxypropyl starch; and
[20] mixing the hydroxypropyl starch, cellulose ether, a dispersion enhancer, and a rheological stabilizer to obtain the modified hydroxypropyl starch.
[21] Preferably, the alkalizing temperature is 15 - 30°C, and the alkalizing time is 1 -2h;
[22] the temperature for the etherification crosslinking reaction is 30 - 90°C, and the time therefor is 0.5 - 5 h.
[23] Preferably, the mixing mode is sirring; the rotating speed for the stirring is 10 - 70 r/min, and the time therefor is 30 - 60 min.
[24] The present invention further provides an application of the modified hydroxypropyl starch in the above technical solution or the modified hydroxypropyl starch prepared by the method in the above technical solution in building materials.
[25] Preferably, the mass percentage of the modified hydroxypropyl starch in the building material is 0.1 - 0.5%.
[26] Compared with the prior art, the present invention has the beneficial effects as follows:
[27] Hydroxypropyl starch in the modified hydroxypropyl starch provided by the present invention contains one or more hydrophilic groups which increase the content of branched substituents and can generate a synergistic effect with straight chain structures of cellulose ether to improve the capabilities of putty, gypsum plaster, glue for tiles, and thermal mortar to hold moisture, so that the putty and the gypsum plaster have excellent water retention capacity, and the opening times of the glue for tiles and the mortar are prolonged; the branched chain structures of the hydroxypropyl starch and one or more of substituents increase the thixotropism of the materials, so that the putty and the gypsum plaster have a rapid thickening property and excellent operating handfeeling and application property; in addition, the straight chains of cellulose ether and one or more of substituents on the branched chains of the hydroxypropyl starch increase the steric hindrance of cement slurry, improve the anti-sliding and anti-sagging properties of the glue for tiles, and improve the dry density and the heat conductivity coefficient of the thermal mortar, and meanwhile, the product dispersed in water forms uniform net structures to further improve the capability of the glue for tiles to hold moisture, which generates an obvious bridging effect to cement particles, endows the mortar body with a larger mechanical anchoring force and improves the tensile adhesive strength of the glue for tiles. Therefore, the obtained modified hydroxypropyl starch can be applied to various building materials: it can improve the application property, the water resistance, and the bonding strength in putty; it can improve the water retention rate, the rupture strength, and the compressive strength in gypsum plaster; it can improve the anti-sliding property, the airing time, and the tensile adhesive strength in glue for tiles; and it can improve the dry density, the heat conductivity coefficient, and the compressive strength in thermal mortar.
[28] Meanwhile, the preparation method provided by the present invention features simple process flow, and can perform etherification reaction and crosslinking reaction at the same time, so that the production efficiency of multi-group crosslinking modified hydroxypropyl starch ether is improved; and with further physical mixed modification through specific doping amounts of cellulose ether, a dispersion enhancer, and a rheological stabilizer to obtain modified hydroxypropyl starch, the product features excellent performance.
[29] Clear and intact description will be made on technical scheme in the embodiment of the present invention below. The described embodiments are merely a part of embodiments of the present invention and are not all the embodiments. On a basis of the embodiments in the present invention, all other embodiments obtained by those skilled in the technical field without creative efforts fall into the scope of protection of the present invention.
[30] Example 1
[31] 100 parts of starch, 10 parts of sodium hydroxide, 10 parts of sodium sulfate, 50 parts of ethanol, 20 parts of an etherifying agent epoxypropane, 10 parts of an etherifying agent sodium chloroacetate, and 0.05 part of epoxy chloropropane were added into a reaction kettle for alkalizing at 20°C for 70 min; the temperature was raised to 55°C and was kept for 1.2 h; the temperature was raised to 75°C and was kept for 1.6 h; a vacuum pump was started; and a solvent was recovered for 2 h at a temperature of 85°C to obtain modified hydroxypropyl starch; and
[32] 5 kg of hydroxypropyl starch, 93 kg of hydroxyethylmethylcellulose, 1.5 kg of polyvinyl alcohol, and 0.5 kg of flaxseed gum were added into a mixer for mixing and stirring for 50 min at the rotating speed of 10 r/min to obtain the modified hydroxypropyl starch.
[33] Example 2
[34] 110 parts of starch, 9 parts of sodium hydroxide, 9 parts of sodium sulfate, 45 parts of ethanol, 18 parts of an etherifying agent epoxypropane, 9 parts of an etherifying agent sodium chloroacetate, and 0.06 part of epoxy chloropropane were added into a reaction kettle for alkalizing at 22°C for 70 min; the temperature was raised to 50°C and was kept for 1.5 h; the temperature was raised to 80°C and was kept for 1.5 h; a vacuum pump was started; and a solvent was recovered for 1.5 h at a temperature of 85°C to obtain modified hydroxypropyl starch; and
[35] 20 kg of hydroxypropyl starch, 74 kg of hydroxyethylmethylcellulose, 5 kg of sodium alginate, and 1 kg of carrageenan were added into a mixer for mixing and stirring for 45 min at the rotating speed of 50 r/min to obtain the modified hydroxypropyl starch.
[36] Comparative example 1
[37] Modified hydroxypropyl cellulose starch is prepared according to the technical solution in the example 1. The difference only lies in that epoxy chloropropane is not added.
[38] Test example 1
[39] Putty performance tests: ground calcium carbonate, ash calcium, and modified hydroxypropyl starch were put in a mixer at a mass ratio of 800: 200: 4 for uniform mixing, water accounting for 40% of the total weight of the components was added, the mixture was stirred by a stirring device and a stirring method specified in /ndoor Putty
Jor Buildings according to standard JG/T298-2010, and then performance tests (application property, water resistance, bonding strength, and water-resistant bonding strength) were carried out according to the standard, with test results shown in table 1.
[40] Table 1 Putty performance tests in examples 1-2 and comparative example 1
Bonding
Standard
Lo } strength (MPa)
Application Water bonding after property resistance strength oo immersion in (MPa) water
No bubbles, / cracks and
No barrier to /
Example 1 obvious 0.85 0.53 scrape coating duslting within 48 h
No bubbles, / cracks and
Example 2 Barnier-free © obvious 0.77 0.49 scrape coating duslting within 48 h - : EE duslting 0.37 0.29
Example 1 scrape coating appear
[41] It can be known from table 1 that the modified hydroxypropyl starch provided by the present invention has the performance of improving the application property, water resistance and bonding strength, where the application property (no barrier to scrape coating), the water resistance (no bubbles, cracks and obvious duslting within 48 h), the standard bonding strength (20.5Mpa), and the bonding strength after immersion in water (>0.3Mpa) meet the requirements on water-resistant putty in the Indoor Putty for Buildings JG/T298-2010, and all are superior to those in the comparative examples.
[42] Test example 2
[43] Gypsum plaster performance tests: flue gas desulfurization gypsum, ground calcium carbonate, glass beads, a retarder, and modified hydroxypropyl starch were put in a mixer at a mass ratio of 660: 280: 60: 2.5: 2.5 for uniform mixing, water accounting for 60% of the total weight of the components was added, the mixture was stirred by a stirring device and a stirring method specified in Gypsum Plaster according to standard
GB/T28627-2012, and then performance tests (initial setting time, final setting time, water-retention rate, rupture strength, and compressive strength) were carried out according to the standard, with test results shown in table 2.
[44] Table 2 Gypsum plaster performance tests in examples 1-2 and comparative example 1
Initial Final Water- Rupture Compressive setting setting retention strength strength time (h) time (h) rate (%) (MPa) (MPa)
Rew Gs ow |e | wi el TT
[45] It can be known from table 2 that the modified hydroxypropyl starch provided by the present invention has the performance of improving the water-retention rate, the rupture strength and the compressive strength of the gypsum plaster, where the water- retention rate (275%), the rupture strength (>2.0Mpa), and the compressive strength (24.0Mpa) meet the requirements on bottom gypsum plaster in Gypsum Plaster
GB/T28627-2012, and all are superior to those in the comparative examples.
[46] Test example 3
[47] Glue for tiles performance tests: cement, fine sand, ground calcium carbonate, a butadiene-styrene rubber powder, a water reducer, calcium formate, and modified hydroxypropyl starch were put in a mixer at a mass ratio of 360: 582: 20: 30: 1: 3: 4 for uniform mixing, water accounting for 25% of the total weight of the components was added, the mixture was stirred by a stirring device and a stirring method specified in
Adhesive for Ceramic Tiles according to standard JC/T547-2017, and then performance tests (sliding, tensile adhesive strength, tensile adhesive strength after immersion in water, tensile adhesive strength after thermal ageing, tensile adhesive strength after freezing and thawing cycle, and tensile adhesive strength after airing for 30 min) were carried out according to the standard, with test results shown in table 3.
[48] Table 3 Glue for tiles performance tests in examples 1-2 and comparative example 1
Tensile
Tensile Tensile | adhesive | Tensile
Tensile adhesive | adhesive | strength | adhesive strength strength after strength
Slide | adhesive after after freezing after (mm) strength immersion | thermal and airing for (MPa) in water ageing thawing 30 min (MPa) (MPa) cycle (MPa) (MPa)
CE TE | |i we [TT
[49] It can be known from table 3 that the modified hydroxypropyl starch provided by the present invention has the performance of improving the anti-sliding property, the air time, and the tensile adhesive strength, where the tensile adhesive strength, the tensile adhesive strength tensile adhesive strength after immersion in water, the tensile adhesive strength after thermal ageing, and the tensile adhesive strength after freezing and thawing cycle(>1.0Mpa), the anti-sliding property (<0.5), and the tensile adhesive strength after airing for 30 min (20.5Mpa) meet the requirements on C2TE glue for tiles in Adhesive for Ceramic Tiles JC/T547-2017, and all are superior to those in the comparative examples.
[50] Test example 4
[51] Thermal mortar performance tests: cement, glass beads, coal ash, a glue powder, polypropylene fiber, and modified hydroxypropyl starch were put in a mixer at a mass ratio of 160: 140: 40: 3.5: 0.5: 1 for uniform mixing, water 1.2 times in amount was added, the mixture was stirred by a stirring device and a stirring method specified in
Thermal Mortar for Buildings according to standard GB/T20473-2021, and then performance tests (dry density, heat conductivity coefficient, and compressive strength) were carried out according to the standard, with test results shown in table 4.
[52] Table 4 Thermal mortar performance tests in examples 1-2 and comparative example 1
Dry density Heat conductivity Compressive (kg/m?) coefficient strength (MPa) (W/mK)
Eee [wwe aw er |e 350 0.0072 0.51
[533] It can be known from table 4 that the modified hydroxypropyl starch provided by the present invention has the performance of improving the dry density, the heat conductivity coefficient, and the compressive strength of the thermal mortar, where the dry density (<350kg/m*), the heat conductivity coefficient (<0.070W/ms+K), and the compressive strength (20.5Mpa) meet the requirements on performance of hardened type I thermal mortar in Thermal Mortar for Buildings GB/T20473-2021, and all are superior to those in the comparative examples.
[54] The above tests show that the process and equipment are simple, easy to operate, free of discharge of three wastes, and green and environmental-friendly. The obtained modified hydroxypropyl starch product features stable quality, can improve the application property, the water resistance, and the bonding strength in putty, can improve the water retention rate, the rupture strength, and the compressive strength in gypsum plaster, can improve the anti-sliding property, the airing time, and the tensile adhesive strength in glue for tiles, and can improve the dry density, the heat conductivity coefficient, and the compressive strength in thermal mortar, which meets the requirements of clients.
The above description of the disclosed embodiments enables professionals skilled in the art to achieve or use the present invention. Various modifications to the embodiments are readily apparent to professionals skilled in the art, and the general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of the present invention. Therefore, the present invention will not be limited to the embodiments shown herein, but falls within the widest scope consistent with the principles and novel features disclosed herein.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107502227A (en) * | 2017-08-30 | 2017-12-22 | 广州市高士实业有限公司 | A kind of non-ionic starch based adhesive and preparation method thereof |
| CN110590966A (en) | 2019-10-28 | 2019-12-20 | 山东一滕新材料股份有限公司 | A kind of preparation method of the modified starch ether that improves the sliding performance of tile adhesive |
| CN113150176A (en) | 2021-04-27 | 2021-07-23 | 山东光大赛路新材料科技有限公司 | Preparation method of multi-group cross-linked modified hydroxypropyl starch ether |
| CN113444185A (en) | 2020-03-24 | 2021-09-28 | 上海钰丽新材料科技有限公司 | High-viscosity hydroxypropyl starch ether and preparation method thereof |
| US20220348801A1 (en) * | 2020-07-09 | 2022-11-03 | Shandong Eton New Material Co., Ltd | Modified hydroxypropyl methyl cellulose for enhanced ceramic tile adhesive and preparation method and application thereof |
| CN115850805A (en) * | 2023-02-27 | 2023-03-28 | 山东一滕新材料股份有限公司 | Multipurpose modified hydroxypropyl starch for building materials as well as preparation method and application thereof |
-
2023
- 2023-09-13 NL NL2035788A patent/NL2035788B1/en active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107502227A (en) * | 2017-08-30 | 2017-12-22 | 广州市高士实业有限公司 | A kind of non-ionic starch based adhesive and preparation method thereof |
| CN110590966A (en) | 2019-10-28 | 2019-12-20 | 山东一滕新材料股份有限公司 | A kind of preparation method of the modified starch ether that improves the sliding performance of tile adhesive |
| EP3816194A1 (en) * | 2019-10-28 | 2021-05-05 | Shandong Eton New Material Co., Ltd. | Preparation method of modified starch ether for improving anti-sliding property of ceramic tile adhesive |
| CN113444185A (en) | 2020-03-24 | 2021-09-28 | 上海钰丽新材料科技有限公司 | High-viscosity hydroxypropyl starch ether and preparation method thereof |
| US20220348801A1 (en) * | 2020-07-09 | 2022-11-03 | Shandong Eton New Material Co., Ltd | Modified hydroxypropyl methyl cellulose for enhanced ceramic tile adhesive and preparation method and application thereof |
| CN113150176A (en) | 2021-04-27 | 2021-07-23 | 山东光大赛路新材料科技有限公司 | Preparation method of multi-group cross-linked modified hydroxypropyl starch ether |
| CN115850805A (en) * | 2023-02-27 | 2023-03-28 | 山东一滕新材料股份有限公司 | Multipurpose modified hydroxypropyl starch for building materials as well as preparation method and application thereof |
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