CN101538019A - Method for preparing hydrophobic nanometer hydrotalcite - Google Patents
Method for preparing hydrophobic nanometer hydrotalcite Download PDFInfo
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- CN101538019A CN101538019A CN200910020585A CN200910020585A CN101538019A CN 101538019 A CN101538019 A CN 101538019A CN 200910020585 A CN200910020585 A CN 200910020585A CN 200910020585 A CN200910020585 A CN 200910020585A CN 101538019 A CN101538019 A CN 101538019A
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- hydrotalcite
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Abstract
The invention relates to a method for preparing hydrophobic nanometer hydrotalcite. The hydrophobic nanometer hydrotalcite with Mg<2+>/Al<3+> of which the molar ratio is 2-3:1 is prepared by adopting a coprecipitation method by adding eunatrol, and leached by using methylbenzene under the action of a phase transfer agent. The hydrophobic nanometer hydrotalcite can be mixed with calcium stearate and zinc stearate and then is added with a lubricating agent, a surfaction agent and an auxiliary stabilizing agent to prepare a composite heat stabilizing agent for hydrophobic nanometer hydrotalcite base PVC. The hydrophobic nanometer hydrotalcite prepared by the method has better hydrophobicity and good compatibility with PVC matrixes, can be used as a stabilizing agent for processing plastics such as PVC, and the like and has the characteristics of no easy separation and good stabilizing effect. The addition of the hydrophobic nanometer hydrotalcite can reduce the balancing torque, improve the processing performance and reduce the cost.
Description
Technical field
The present invention relates to a kind of preparation that is used for hydrophobic nanometer hydrotalcite polyvinyl chloride, that have long-acting thermostability.
Background technology
As everyone knows, PVC easily decomposes under the processing temperature condition, must add stablizer and just can make its smooth processing.In addition, polyvinyl chloride is heated or when being subjected to ultraviolet radiation, also can causing the degraded of polymkeric substance and take off HCl.Therefore, PVC's uses and processes and must use stablizer.Stablizer is a kind of chemical assistant, and it can suppress degraded and the variable color that PVC causes owing to heat, light action in machine-shaping and use.Stablizer can be divided into base lead salt stablizer, metallic soap class, organo-tin compound, organic stabilizer and one package stabilizer five big classes by its chemical structure.
Because advantages such as the lead salt stabilizer raw material is easy to get, production technique is simple, cheap, performance is outstanding are still most widely used kind so far, output accounts for 65% of China's stablizer output.The shortcoming of lead salt stabilizer is toxicity height, coloring plastic difficulty, the bad dispersibility in plastics etc., and particularly the powdery lead compound produces a large amount of lead salt dust in batching, stirring or plasticizing process, can produce greatly harm to operator and environment.In order to overcome these shortcomings, adopt complex lead salt stabilizer mostly.Complex lead salt stabilizer is compared with traditional three salt, disalt, and performance improves a lot, and it with strong points, simple to operate reduced the processing technology that is mixed, thereby reduced dust pollution, reduced cost.In a word, complex lead salt stabilizer is celebrated with its excellent combination property.
(Layered Double Hydrotalcides is the negatively charged ion stratiform functional inorganic materials that a class has laminate structure LDHs) to hydrotalcite, but has chemical constitution and the particular structure and the performance of modulation.Its typical magnalium hydrotalcite chemical formula is: [Mg6Al2 (OH) 16CO3] 4H2O.The hydrotalcite tool integrates all multi-functional fillings and improved starting material such as fire retardant, insulating compound, stablizer, tinting material, surface slip agent, antiaging agent, anti UV agent.The performance of hydrotalcite: (1) magnalium hydrotalcite is the good environment friendly flame retardant of efficient, nontoxic, low cigarette, high performance-price ratio.Hydrotalcite has magnesium hydroxide and similar structure of aluminium hydroxide and composition concurrently, discharges a large amount of water and carbonic acid gas during decomposes, and absorbs a large amount of heat, can reduce the temperature of combustion system; Decompose water vapor and the dilution of carbon dioxide gas physical efficiency that discharges and intercept inflammable gas; The carbide that forms when magnesium aluminum oxide that thermolysis generates and macromolecular material burning forms protective membrane at material surface, thereby has intercepted the further intrusion of oxygen, also plays flame retardant effect.Solid product after hydrotalcite particle is decomposed has very big specific surface area and very strong alkalescence, and sour gas and the smog that discharges during absorbing material thermolysis in time also is transformed into corresponding compounds, thereby plays the effect that presses down cigarette and smoke elimination.Therefore hydrotalcite is the nontoxic halogen-free flame retardants new variety of environment amenable Smoke Suppression that get a good chance of.Its flame retardant properties obviously is better than aluminium hydroxide and magnesium hydroxide, and has both advantages concurrently.(2) hydrotalcite is nontoxic heat stable material.LDHs can be used as efficient, nontoxic, the inexpensive thermo-stabilizer of polyvinyl chloride (PVC).It can absorb PVC effectively and decompose the HCl that produces in processing and use, improves processing conditions and the thermostability of PVC.Can with organotin or plumbous zinc jointly as thermo-stabilizer, or use jointly with other auxiliary agents, further improve the thermostability of PVC.LDHs itself is nontoxic, can replace lead salt and other metal species stablizers on a large scale, and can be used among the food product pack PVC.(3) hydrotalcite and other preparation are used with, except the thermotolerance that can improve macromolecular material, can also improve their other performance.As physical strength, anti-aging temperature, product surface brightness, insulating property, antistatic property, anti-ultraviolet property etc.Hydrotalcite also has good thermal insulation, promotes the PVC plastic sheeting for farm use to ultrared absorption, improves the heat retaining property of plastic sheeting for farm use.The purposes of hydrotalcite: (1) is as multi-functional filling improving agents such as fire-retardant, stable, the insulation of macromolecular materials such as plastics, rubber, chemical fibre, painted, uvioresistants.(2) as dyestuff, coating, paint, printing ink, makeup daily-use chemical industry starting material.(3) as dyeing and weaving thing waste water conditioner, radioactive wastewater treatment agent, removing pollutant flocculation agent.(4) as chemical catalyst carrier and aromatized catalyst.(5) as the improving agent and the intermediate of multiple material.
Nano hydrotalcite has high specific surface, and the more conventional hydrotalcites of performance such as its flame retardant resistance, adsorptivity, stability all have remarkable lifting, are a kind of very promising functional materials.Existing many about the patent of nano hydrotalcite preparation, as " a kind of is the method (patent No. ZL 03150037.4) of feedstock production nano level magnesium aluminum-hydrotalcite with bittern ", after this patent removes the processing of impurity and coloring matter with industrial bittern, utilize magnesium salts wherein to prepare nano hydrotalcite, can suitably reduce the production cost of hydrotalcite; Patent " the chloride superpolymer composite thermal stabilizer of a kind of hydrotalcite (patent No. ZL200410037656.7) " mainly is to have prepared nano hydrotalcite, and has synthesized the PVC composite thermal stabilizer with hydrotalcite and calcium soap, the zinc soap of preparation.
The preparation method of existing multiple nano hydrotalcite, but the hydrotalcite of preparation is hydrophilic.Organic substance consistencies such as hydrophilic hydrotalcite and polyvinyl chloride are bad, are difficult to uniform mixing, and easily separate out, and make that the one package stabilizer stabilising effect is undesirable, greatly limited the effect of hydrotalcite in the PVC composite thermal stabilizer.
Summary of the invention
Technical problem to be solved by this invention provides a kind of preparation method of hydrophobic nanometer hydrotalcite, and prepared hydrophobic nanometer hydrotalcite is good with the organic substance consistency, easily disperses, and prepared one package stabilizer stabilising effect is good.
Hydrophobic nanometer hydrotalcite used in the present invention is that interlayer anion is the magnesium aluminum-hydrotalcite of carbonate: wherein, and Mg
2+/ Al
3+Mol ratio satisfies 2～3: 1.Concrete preparation method: preparation 2 * 10
-3Mol/l aqueous solution sodium oleate (solution A), with magnesium salts and aluminium salt in molar ratio 2～3: 1 mixed be mixed with Mg
2+Concentration is the aqueous solution (solution B) of 0.3～0.6mol/L, with KOH or NaOH and Na
2CO
3Or K
2CO
3Press OH-/CO
3 2-Mol ratio 12～16: 1 mixed obtain solution (solution C), wherein, CO
3 2-Concentration will keep CO
3 2-/ Al
3+Mol ratio is 1: 2.Get the 500ml solution A and put into the 2L three-necked flask, heating in water bath to 40～60 ℃, under the condition of vigorous stirring (more than the 120rpm), (400～500ml) solution B and solution C, rate of addition is for dropwising in 30～45min to drip equal volume simultaneously.The pH value of solution value remains on 9.0～9.5 in the dropping process.Dropwise and continue to stir 30min, bath temperature to the 60～80 ℃ insulation 2～3h that raises then naturally cools to room temperature, repeatedly suction filtration, washing precipitation to the pH value 7～8.Precipitation dissolving again, add 10～20g NaH
2PO
4With 200ml toluene, standing demix behind the vigorous stirring 30min, precipitation is transferred to toluene.Discard lower aqueous solution, toluene is removed in distillation, has both got hydrophobic nanometer hydrotalcite.
The hydrotalcite particle diameter of present method preparation is 30～70nm.
The present invention adopts the method for co-precipitation, add sodium oleate and prepare Mg: the Al mol ratio is 2～3: 1 hydrophobic nanometer hydrotalcite, under the consisting of phase-transferring agent effect, use toluene that hydrophobic nanometer hydrotalcite is extracted, mix with calcium stearate, Zinic stearas, add lubricant, surface modifier and auxiliary stabilizer again and can be made into composite heat stabilizer for hydrophobic nano-hydrotalcite PVC.
Utilize the prepared hydrophobic nanometer hydrotalcite of the present invention, be mixed with the one package stabilizer that following quality is formed:
Calcium stearate 20～40%
Zinic stearas 15～25%
Hydrophobic nanometer hydrotalcite 10～30%
Lubricant 5～15%
Surface modifier 4～7%
Auxiliary heat stabilizer 5～15%
Above percentage ratio is mass percent.Lubricant mainly contains polyethylene wax, Tegin 55G or stearic acid; Surface modifier mainly contains pentaerythritol ester or triphenyl phosphite; Auxiliary stabilizer mainly contains epoxy soybean oil or diphenylpropane-1,3-dione(DPPO).
Concrete hybrid mode is as follows:
Earlier calcium stearate, Zinic stearas and hydrotalcite are added thorough mixing in the reactor.Get mixture, add heating and stirring in the kneader, add surface modifier, mediate 20min down at 100～110 ℃, in kneader, add lubricant then, auxiliary heat stabilizer, mediate and stir 30min, discharging compressing tablet, screening, packing had both got the finished product.
Advantage of the present invention:
Evenly (30～70nm), hydrophobic effect is good, and is good with the organic solvent mutual solubility for the prepared nano hydrotalcite size distribution of the present invention.Detect with X-ray diffractometer, the result shows that product has very high degree of crystallinity.
Unusual effect of the present invention is: prepared hydrophobic nanometer hydrotalcite is as the stablizer of plastic working such as PVC, have be difficult for separating out, characteristics that stabilising effect is good; Balancing torque when the hydrophobic nanometer hydrotalcite that adds the present invention's preparation can reduce PVC and prepares improves processing characteristics, reduces cost.By the PVC that adds the hydrophobic nano-hydrotalcite composite thermal stabilizer being carried out the static-aging experiment, the result shows, adds the thermostability that one package stabilizer of the present invention can obviously improve PVC.Under 180 ± 1 ℃ of conditions, PVC not only has good initial coloring, and its heat-stable time has also reached more than 120～200min.Preparation method of the present invention is pollution-free, energy consumption is low.
Embodiment
Embodiment 1:
Preparation 2 * 10
-3Mol/l aqueous solution sodium oleate (solution A) takes by weighing 98.59g MgSO respectively
47H
2O and 66.64gAl
2(SO
4)
318H
2O is dissolved in the 500ml deionized water and is mixed with Mg
2+And Al
3+2: 1 in molar ratio mixing solutions (solution B) is with 48.00g NaOH and 10.60g Na
2CO
3Be dissolved in the 500ml deionized water and be mixed with OH
-/ CO
3 2-12: 1 mixing solutions of mol ratio (solution C).Get the 500ml solution A and put into the 2L three-necked flask, heating in water bath to 40～60 ℃, under intense stirring condition, Dropwise 5 00ml solution B and 500ml solution C simultaneously, rate of addition is for dropwising in 45min.The pH value of solution value remains on 9.0～9.5 in the dropping process.Dropwise and continue to stir 30min, bath temperature to the 60～80 ℃ insulation 3h that raises then naturally cools to room temperature, repeatedly suction filtration, washing precipitation to the pH value 7～8.Precipitation dissolving again, add 20g NaH
2PO
4With 200ml toluene, standing demix behind the vigorous stirring 30min, precipitation is transferred to toluene.Discard lower aqueous solution, toluene is removed in distillation, both the magnalium ratio is 2: 1 a hydrophobic nanometer hydrotalcite.The hydrotalcite particle diameter of preparation is 30～50nm.
Embodiment 2:
According to the preparation process of embodiment 1, take by weighing 147.89g MgSO
47H
2O and 66.64g Al
2(SO
4)
318H
2O is dissolved in the 500ml deionized water and is mixed with Mg2+ and 3: 1 in molar ratio mixing solutions of Al3+ (solution B), with 64.00gNaOH and 10.60g Na
2CO
3Be dissolved in the 500ml deionized water and be mixed with OH
-/ CO
3 2-16: 1 mixing solutions of mol ratio (solution C).Step as stated above makes the magnalium mol ratio and is 3: 1 hydrophobic nanometer hydrotalcite.The hydrotalcite particle diameter of preparation is 30～70nm.
Hydrotalcite with embodiment 1 and 2 preparations mixes with calcium stearate, Zinic stearas, lubricant, surface modifier and auxiliary heat stabilizer respectively, and concrete hybrid mode is as follows:
Earlier calcium stearate (30 parts), Zinic stearas (20 parts) and hydrotalcite (20 parts) are added thorough mixing in the reactor.Get mixture, add heating and stirring in the kneader, add surface modifier (5 parts), mediate 20min down at 100～110 ℃, add lubricant (10 parts) then in kneader, auxiliary heat stabilizer (15 parts) is mediated and is stirred 30min, discharging compressing tablet, screening, packing had both got the finished product.
Wherein: lubricant is selected from polyethylene wax, Tegin 55G or stearic acid and all can; Surface modifier is selected pentaerythritol ester or triphenyl phosphite; Auxiliary heat stabilizer is selected epoxy soybean oil or diphenylpropane-1,3-dione(DPPO).
Above-mentioned two kinds of one package stabilizers are added respectively among the 100 mass parts PVC, add 60 mass parts dimixo-octyl phthalates (DOP) again, descended mixing 10 minutes at 140 ℃, be pressed into the thin slice that thickness is 1mm under 100 ℃, be cut into the test piece of 1cm * 1cm, do the static-aging experiment under 180 ± 1 ℃ of conditions, experimental result sees Table 1.Wherein embodiment 3 is a Comparative Examples.
Table 1
| Embodiment | Mg 2+/Al 3+ | PVC (part) | DOP (part) | Composite thermal stabilizer (part) | Heat-stable time (minute) |
| 1 | 2 | 100 | 60 | 3 | 175 |
| 2 | 3 | 100 | 60 | 3 | 193 |
| 3 | / | 100 | 60 | 0 | 7 |
Embodiment 4～5:
Use 2: 1 hydrophobic nanometer hydrotalcite of Mg/Al mol ratio, change the composition and the ratio of composite thermal stabilizer, add among 100 parts of PVC by same amount, add 60 parts of dimixo-octyl phthalates (DOP) again, then by GB GB2113-82 " plastics whiteness experimental technique ", three kinds of PVC plastics of preparation are carried out heat-resisting whiteness experiment, table 2 is three kinds of composite thermal stabilizer compositing formulas, and table 3 is that being placed on test piece with whiteness is the relative whiteness value of testing in the whiteness instrument checked of 85% standard white body.Can find that from table 3 prepared hydrophobic nanometer hydrotalcite one package stabilizer is compared with traditional stablizer, has outstanding thermostability.
Table 2
| Embodiment | Hydrophobic nanometer hydrotalcite (part) | Calcium stearate (part) | Zinic stearas (part) | Modification agent+lubricant+auxiliary stabilizer (part) |
| 1 | 20 | 30 | 20 | 5+10+15 |
| 4 | 10 | 36 | 24 | 5+10+15 |
| 5 | 30 | 24 | 16 | 5+10+15 |
Wherein: lubricant is selected from polyethylene wax, Tegin 55G or stearic acid and all can; Surface modifier is selected pentaerythritol ester or triphenyl phosphite; Auxiliary heat stabilizer is selected epoxy soybean oil or diphenylpropane-1,3-dione(DPPO).
Table 3
Claims (3)
1, a kind of preparation method of hydrophobic nanometer hydrotalcite is characterized in that comprising the steps:
(1) obtain solution A:2 * 10
-3The aqueous solution sodium oleate of mol/l;
(2) obtain solution B: with magnesium salts and aluminium salt in molar ratio 2～3: 1 mixed be mixed with Mg
2+Concentration is the aqueous solution of 0.3～0.6mol/L;
(3) obtain solution C: with KOH or Na0H and Na
2CO
3Or K
2CO
3Press OH
-/ CO
3 2-Mol ratio 12～16: 1 mixed obtain solution C;
(4) get the 500ml solution A and put into the 2L three-necked flask, heating in water bath to 40～60 ℃, under intense stirring condition, drip solution B and the solution C of 400～500ml simultaneously, rate of addition is for dropwising in 30～45min, the pH value of solution value remains on 9.0～9.5 in the dropping process, dropwise and continue to stir 30min, bath temperature to 60～80 ℃ insulation 2～3h then raises, naturally cool to room temperature, repeatedly suction filtration, washing precipitation to the pH value 7～8, precipitation dissolving again, add 10～20g NaH
2PO
4With 200ml toluene, standing demix behind the vigorous stirring 30min, precipitation is transferred to toluene, discards lower aqueous solution, and toluene is removed in distillation, has both got hydrophobic nanometer hydrotalcite.
2, the preparation method of hydrophobic nanometer hydrotalcite according to claim 1 is characterized in that described magnesium salts and aluminium salt are respectively vitriol or muriate or nitrate.
3, the preparation method of hydrophobic nanometer hydrotalcite according to claim 1 is characterized in that the hydrophobic nanometer hydrotalcite particle diameter that obtains is 30～70nm.
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|---|---|---|---|
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|---|---|---|---|
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| CN101538019B CN101538019B (en) | 2011-04-20 |
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Cited By (12)
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|---|---|---|---|---|
| CN102504339A (en) * | 2011-10-25 | 2012-06-20 | 浙江海普顿新材料股份有限公司 | Powdery calcium-zinc complex heat stabilizer and preparation method and application thereof |
| CN102643494A (en) * | 2012-05-10 | 2012-08-22 | 唐山师范学院 | Preparation method and applications of calcium/zinc composite thermal stabilizing additive used for polyvinyl chloride |
| CN103709551A (en) * | 2013-12-06 | 2014-04-09 | 上海特种电线电缆（集团）有限公司 | High-temperature resistant fireproof nano insulating material |
| CN104169219A (en) * | 2012-03-26 | 2014-11-26 | 协和化学工业株式会社 | Fine hydrotalcite particles |
| CN104231317A (en) * | 2014-08-21 | 2014-12-24 | 安徽吉安特种线缆制造有限公司 | Modified talcum for anti-aging chlorinated polyethylene cable material and preparation method thereof |
| CN104710649A (en) * | 2015-03-24 | 2015-06-17 | 宁波高新区零零七工业设计有限公司 | Method for preparing hydrotalcite heat stabilizer |
| CN105694296A (en) * | 2016-04-15 | 2016-06-22 | 佛山市聚成生化技术研发有限公司 | Preparation method of tri-element supramolecular mixed polyvinyl chloride heat stabilizer and stabilizer prepared by same |
| CN106317461A (en) * | 2016-08-23 | 2017-01-11 | 深圳市志海实业股份有限公司 | Synthesis preparation method of intercalation polymerization efficient nontoxic environment-friendly calcium-zinc stabilizer |
| CN106745118A (en) * | 2016-12-30 | 2017-05-31 | 洛阳中超新材料股份有限公司 | A kind of magnalium hydrotalcite and the method for preparing magnalium hydrotalcite |
| CN107190255A (en) * | 2017-04-11 | 2017-09-22 | 中国科学院上海硅酸盐研究所 | A kind of super-hydrophobic magnesium or magnesium alloy materials and its preparation method and application |
| CN110306336A (en) * | 2019-06-26 | 2019-10-08 | 东莞职业技术学院 | A kind of production technology of flame retardant knitted cloth |
| CN112280100A (en) * | 2020-10-13 | 2021-01-29 | 裕克施乐塑料制品（太仓）有限公司 | Composite intumescent flame retardant and preparation method thereof |
Family Cites Families (2)
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|---|---|---|---|---|
| US5079203A (en) * | 1990-05-25 | 1992-01-07 | Board Of Trustees Operating Michigan State University | Polyoxometalate intercalated layered double hydroxides |
| CN1962453A (en) * | 2006-11-22 | 2007-05-16 | 天津化工研究设计院 | Process for producing hydrotalcite-like layered hydroxide |
-
2009
- 2009-04-24 CN CN2009100205852A patent/CN101538019B/en not_active Expired - Fee Related
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| CN102504339A (en) * | 2011-10-25 | 2012-06-20 | 浙江海普顿新材料股份有限公司 | Powdery calcium-zinc complex heat stabilizer and preparation method and application thereof |
| CN104169219B (en) * | 2012-03-26 | 2016-02-10 | 协和化学工业株式会社 | Fine hydrotalcite particle |
| CN104169219A (en) * | 2012-03-26 | 2014-11-26 | 协和化学工业株式会社 | Fine hydrotalcite particles |
| CN102643494A (en) * | 2012-05-10 | 2012-08-22 | 唐山师范学院 | Preparation method and applications of calcium/zinc composite thermal stabilizing additive used for polyvinyl chloride |
| CN103709551A (en) * | 2013-12-06 | 2014-04-09 | 上海特种电线电缆（集团）有限公司 | High-temperature resistant fireproof nano insulating material |
| CN104231317A (en) * | 2014-08-21 | 2014-12-24 | 安徽吉安特种线缆制造有限公司 | Modified talcum for anti-aging chlorinated polyethylene cable material and preparation method thereof |
| CN104710649A (en) * | 2015-03-24 | 2015-06-17 | 宁波高新区零零七工业设计有限公司 | Method for preparing hydrotalcite heat stabilizer |
| CN105694296A (en) * | 2016-04-15 | 2016-06-22 | 佛山市聚成生化技术研发有限公司 | Preparation method of tri-element supramolecular mixed polyvinyl chloride heat stabilizer and stabilizer prepared by same |
| CN106317461A (en) * | 2016-08-23 | 2017-01-11 | 深圳市志海实业股份有限公司 | Synthesis preparation method of intercalation polymerization efficient nontoxic environment-friendly calcium-zinc stabilizer |
| CN106745118A (en) * | 2016-12-30 | 2017-05-31 | 洛阳中超新材料股份有限公司 | A kind of magnalium hydrotalcite and the method for preparing magnalium hydrotalcite |
| CN107190255A (en) * | 2017-04-11 | 2017-09-22 | 中国科学院上海硅酸盐研究所 | A kind of super-hydrophobic magnesium or magnesium alloy materials and its preparation method and application |
| CN107190255B (en) * | 2017-04-11 | 2019-04-16 | 中国科学院上海硅酸盐研究所 | A kind of super-hydrophobic magnesium or magnesium alloy materials and its preparation method and application |
| CN110306336A (en) * | 2019-06-26 | 2019-10-08 | 东莞职业技术学院 | A kind of production technology of flame retardant knitted cloth |
| CN112280100A (en) * | 2020-10-13 | 2021-01-29 | 裕克施乐塑料制品（太仓）有限公司 | Composite intumescent flame retardant and preparation method thereof |
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