CN103834055B - A kind of low-temperature environment-friendly whipping agent - Google Patents
A kind of low-temperature environment-friendly whipping agent Download PDFInfo
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- CN103834055B CN103834055B CN201410104864.8A CN201410104864A CN103834055B CN 103834055 B CN103834055 B CN 103834055B CN 201410104864 A CN201410104864 A CN 201410104864A CN 103834055 B CN103834055 B CN 103834055B
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- coagent
- whipping agent
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
- C08J9/06—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent
- C08J9/10—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent developing nitrogen, the blowing agent being a compound containing a nitrogen-to-nitrogen bond
- C08J9/102—Azo-compounds
- C08J9/103—Azodicarbonamide
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2203/00—Foams characterized by the expanding agent
- C08J2203/04—N2 releasing, ex azodicarbonamide or nitroso compound
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2327/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers
- C08J2327/02—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment
- C08J2327/04—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment containing chlorine atoms
- C08J2327/06—Homopolymers or copolymers of vinyl chloride
Abstract
The invention provides a kind of low-temperature environment-friendly whipping agent, by AC? whipping agent 40 ~ 80 parts, coagent 10 ~ 40 parts, decomposition control agent 1 ~ 10 part, methane amide remover 5 ~ 20 parts composition, wherein, coagent is single coagent A or the mixture of coagent A, B, C three, coagent A is the zinc such as zinc oxide, Zinic stearas compounds, coagent B is surface-treated urea or thiocarbamide, and coagent C is a kind of or several combination in trolamine, tetramethylolmethane, glycerine.Not only decomposition temperature is low for low-temperature environment-friendly whipping agent obtained by the present invention, and meanwhile, degradation production does not contain formaldehyde completely, and, be also substantially devoid of methane amide in degradation production.
Description
Technical field
The invention belongs to chemical foaming agent field, especially a kind of low-temperature environment-friendly whipping agent.
Background technology
AC whipping agent is that a kind of gas forming amount is large, superior performance, broad-spectrum whipping agent.The chemical name of AC whipping agent is Cellmic C 121, and it is widely used in various synthetic materials, and its application spreads all over the industries such as slippers, sole, shoe-pad, plastic wallpaper, top ceiling, flooring laminate, leatheroid, thermal insulation, sound-proof material.Further, due to AC whipping agent have stable performance, nonflammable, do not pollute, nonpoisonous and tasteless, mould do not corroded goods are not dyeed, decomposition temperature is adjustable, do not affect the features such as solidification and shaping speed, it has broad application prospects.
Although AC whipping agent is of many uses, but, there is following shortcoming in existing AC whipping agent (Cellmic C 121): (1) AC foaming agent decomposition temperature is at 200 ~ 208 DEG C, even if add the activator such as zinc oxide, zinc carbonate composition compound foaming agent in AC whipping agent, the decomposition temperature of compound foaming agent is also more than 155 DEG C, and decomposition temperature is high; (2) because the decomposition reaction of AC whipping agent is a violent thermopositive reaction, the decomposition reaction of adding the AC whipping agent caused by zn cpds is too quick, make that decomposition caused heat release is too concentrated, decomposition course is uncontrollable, easily cause the generation of second order reaction, produce some poisonous, noxious products, such as AC whipping agent can produce toxic substance-methane amide when decomposing at higher than the temperature of 160 DEG C, has a strong impact on the healthy of user.The western countries such as European Union propose high requirement (requiring that in goods, formamide content is lower than 10ppm) to the formamide content in foaming product, and adopt methane amide output in the obtained foaming product of common AC whipping agent to be generally 150 ~ 500ppm, also have a strong impact on and govern the export trade of China.
At present, for above-mentioned shortcoming (1), home and abroad have developed the composite modified production of low-temperature foaming agent of a kind of AC, and main raw is AC whipping agent (Cellmic C 121), H whipping agent (dinitrosopentamethlyene tetramine), urea fat.Although the decomposition temperature of the composite modified production of low-temperature foaming agent of this AC is 125 ~ 135 DEG C, because this product contains H whipping agent, H whipping agent can produce another kind of toxic substance-formaldehyde when decomposing, and therefore, H whipping agent is also listed in the row of forbidding chemical by American-European countries.For above-mentioned shortcoming (2), way being is all is being researched and solved in home and abroad, but, also there is not breakthrough.
Summary of the invention
The present invention aims to provide a kind of low-temperature environment-friendly whipping agent that can solve the problems of the technologies described above, and this whipping agent not only decomposition temperature is low, and meanwhile, degradation production does not contain formaldehyde completely, and, be also substantially devoid of methane amide in degradation production.
A kind of low-temperature environment-friendly whipping agent, by AC whipping agent 40 ~ 80 parts, coagent 10 ~ 40 parts, decompose control agent 1 ~ 10 part, methane amide remover 5 ~ 20 parts composition, wherein, coagent is single coagent A or coagent A, B, the mixture of C three, coagent A is to toluenesulfinic acid zinc, benzene sulfinic acid zinc, tosic acid zinc, ZINC P-PHENOLSULFONATE, zinc citrate, zinc lactate, a kind of or several combination in Zinic stearas, coagent B is for using direactive glyceride, stearic acid, in oleic acid any one or severally carry out surface-treated urea or thiocarbamide, coagent C is trolamine, tetramethylolmethane, a kind of or several combination in glycerine, decomposition control agent is a kind of or several combination in hexamethylenetetramine, sodium nitrilo triacetate, nitrilotriacetic acid, sodium ethylene diamine tetracetate, methane amide remover is a kind of or several combination in diethyl malonate, magnesium oxide, magnesium hydroxide, calcium oxide, calcium hydroxide.
Advantageous Effects of the present invention is:
(1) usually AC foaming agent decomposition temperature is reduced by adding the zinc such as zinc oxide, Zinic stearas compounds in prior art, its decomposition temperature is generally more than 155 DEG C, and the present invention is by the selection to coagent, the decomposition temperature of AC whipping agent is made to be reduced to about 135 DEG C, further, the degradation production of coagent is not completely containing formaldehyde;
(2) the present invention decomposes by adding the decomposition rate that control agent slows down AC, decomposition reaction is made to become mild, heat release is even, prevent the too high generation causing a series of second order reaction of local temperature, thus, reduce the generation of poisonous and harmful substances (i.e. methane amide), simultaneously, the decomposition control agent that the present invention adopts is that itself is nontoxic, harmless, and, the chemical substance that its degradation production is also nontoxic;
(3) be the hazardous and noxious substances reduced further in degradation production, goods of guaranteeing to fire are nontoxic, the present invention is by adding some methane amide removers, and, the present invention, by selecting methane amide remover, makes methane amide remover can react with methane amide, thus reaches the object eliminating methane amide, meanwhile, the reaction product ensureing methane amide remover itself and methane amide remover and methane amide is all to human non-toxic, harmless;
(4) the present inventor is through testing many times, obtain the better parameters combination scheme of AC whipping agent, coagent, decomposition control agent, methane amide remover deal, make the low-temperature environment-friendly whipping agent that finally can obtain the discharge of high gas forming amount, low decomposition temperature, zero formaldehyde and low methane amide.
Prepare a method for above-mentioned low-temperature environment-friendly whipping agent, comprise the following steps:
(1) get AC whipping agent 40 ~ 80 parts, coagent 10 ~ 40 parts, decompose control agent 1 ~ 10 part, methane amide remover 5 ~ 20 parts, mix;
(2) comminuting matter;
(3) employing 300 ~ 450 orders sieve to remove and do not pulverize coarse particles completely;
(4) fine particle after thick to grinding screen carries out secondary mixing, obtains low-temperature environment-friendly whipping agent product.
The preparation method of low-temperature environment-friendly whipping agent of the present invention have employed secondary mixing, and the uniformity coefficient of obtained low-temperature environment-friendly whipping agent is higher, makes the function of each moiety of low-temperature environment-friendly whipping agent obtain maximum release; In addition, the present invention is pulverized material by step (2), limits, make the grain diameter of the low-temperature environment-friendly whipping agent obtained by the present invention less to the grain diameter after pulverizing, improve the direct contact area of different components, improve uniformity coefficient further.
The mass ratio of coagent A, B, C is preferably: during 1 ~ 1.5:4:1 ~ 1.5, can reduce below decomposition temperature to 135 DEG C.
In addition, in order to save the cost of coagent of the present invention, make the decomposition temperature of obtained whipping agent minimum, coagent preferably adds 20 ~ 30 parts simultaneously.In order to save the cost of decomposition control agent of the present invention, the amount of methane amide being down to minimum, meanwhile, keeping suitable rate of decomposition, decompose control agent and preferably add 3 ~ 5 parts.In order to save the cost of methane amide remover of the present invention, methane amide remover preferably adds 5 ~ 8 parts.
In specific implementation process, above-mentioned steps (3) preferably adopts micronizer mill to pulverize material, certainly, pulverising step herein also can adopt other grinding mode, such as: mechanical mill etc., but, adopt the pulverizing of micronizer mill fastest, further, be not easy in crushing process to pollute other impurity.
In addition, the pulverising step in above-mentioned steps (2) is preferably and is pulverized to its median size by crushing material is 3 ~ 5 microns, like this, can greatly reduce returning charge rate.
Embodiment
A kind of low-temperature environment-friendly whipping agent, by AC whipping agent 40 ~ 80 parts, coagent 10 ~ 40 parts, decompose control agent 1 ~ 10 part, methane amide remover 5 ~ 20 parts composition, wherein, coagent is single coagent A or coagent A, B, the mixture of C three, coagent A is to toluenesulfinic acid zinc, benzene sulfinic acid zinc, tosic acid zinc, ZINC P-PHENOLSULFONATE, zinc citrate, zinc lactate, a kind of or several combination in Zinic stearas, coagent B is for using direactive glyceride, stearic acid, in oleic acid any one or severally carry out surface-treated urea or thiocarbamide, coagent C is trolamine, tetramethylolmethane, a kind of or several combination in glycerine, decomposition control agent is a kind of or several combination in hexamethylenetetramine, sodium nitrilo triacetate, nitrilotriacetic acid, sodium ethylene diamine tetracetate, methane amide remover is a kind of or several combination in diethyl malonate, magnesium oxide, magnesium hydroxide, calcium oxide, calcium hydroxide.
Prepare a method for above-mentioned low-temperature environment-friendly whipping agent, comprise the following steps:
(1) get AC whipping agent 40 ~ 80 parts, coagent 10 ~ 40 parts, decompose control agent 1 ~ 10 part, methane amide remover 5 ~ 20 parts, close evenly;
(2) adopt micronizer mill comminuting matter, being pulverized to its median size by crushing material is 3 ~ 5 microns;
(3) employing 300 ~ 450 orders sieve to remove and do not pulverize coarse particles completely;
(4) fine particle after thick to grinding screen carries out secondary mixing, obtains low-temperature environment-friendly whipping agent product.
Certainly, above-mentioned steps (2) also can adopt other grinding mode, such as: mechanical mill etc., but, adopt the pulverizing of micronizer mill fastest, and, be not easy in crushing process to pollute other impurity.In addition, crushing material also can only be pulverized as being greater than 5 microns to its median size by the pulverising step in above-mentioned steps (2), but like this, after sieving, coarse particles content is large, and returning charge rate is high.
Because in the formula of low-temperature environment-friendly whipping agent of the present invention, coagent, decomposition control agent and methane amide remover all exist a large amount of array modes, therefore, embodiments of the invention One's name is legion.The applicant has intercepted the index of section Example (embodiment 1 ~ embodiment 22) to obtained low-temperature environment-friendly whipping agent and has measured.In addition, in order to embody coagent of the present invention, decompose the meaning of control agent and the restriction of methane amide remover parameter, the applicant additionally provides 8 comparative examples (contrast 23 ~ contrast 30).Now list embodiments of the invention 1 ~ 22 and contrast 23 ~ 30 one-tenth be grouped into and composition number (table 1 ~ 2, wherein, table 1 lists the deal of AC whipping agent in each embodiment, the moiety of coagent and deal; Table 2 lists moiety and the deal of moiety and deal and the methane amide decomposing control agent in each embodiment).
Table 1
Table 2
By measuring the foaming situation of low-temperature environment-friendly whipping agent of the present invention at each temperature section, determine the minimum blowing temperature of whipping agent, i.e. lowest decomposition temperature.Meanwhile, by the gas forming amount in the analytical unit time, calculate rate of decomposition.Wherein, the concrete measuring method of the gas forming amount of this patent whipping agent is that the gas forming amount testing method provided according to rower (HG/T2097-2008) carries out measuring.
Prepare low-temperature environment-friendly whipping agent according to the method preparing low-temperature environment-friendly whipping agent of the present invention, then adopt this low-temperature environment-friendly whipping agent to carry out pvc material (being called for short " PVC ") injection molding application test.
PVC injection molding application test formula (unit: part)
PVC（SG7）95~110
DOP50~65
Low-temperature environment-friendly whipping agent 1.5 ~ 2.2 of the present invention
Lead sulfate tribasic 1.7 ~ 2.4
Lead stearate 0.8 ~ 1.1
Titanium dioxide 2.0 ~ 3.0
Calcium carbonate 19 ~ 26
Stearic acid 1.0 ~ 1.5
PVC moulded from foam technique: weighed material by formula, banburying 15 minutes in input Banbury mixer, again on opening rubber mixing machine about 80 DEG C open and be smelt sheet, cut-parts take 90 grams of sizing materials, put into vulcanizing press 140 DEG C, foam 10 minutes, after depanning, cool one hour, measure the content of methane amide and formaldehyde.
Now list the test-results (see table 3) of embodiments of the invention 1 ~ 22 and contrast 23 ~ 30:
Table 3
From the embodiment 1 ~ 22 in table 3, low-temperature environment-friendly whipping agent of the present invention is when being down to 128 ~ 140 DEG C by lowest decomposition temperature, also can delay rate of decomposition to 0.61mL/ (gmin), thus, reduce formamide content to below 9.5ppm (meeting the standard of the formamide content in the foaming product of European Union's formulation lower than 10ppm), meanwhile, keep high gas forming amount (159 ~ 179mL/g) and do not produce formaldehyde.Further, when coagent is 20 ~ 30 parts, the lowest decomposition temperature of low-temperature environment-friendly whipping agent sees the minimum level that can maintain 129 ~ 133 DEG C; When to decompose control agent be 3 ~ 5 parts, the amount of methane amide can be maintained≤the level of 4.5ppm.
In addition, from table 1,2, the embodiment 7,8,11 and 12 of 3 and the contrast of other embodiments can find out, when the mass ratio of coagent A, B, C is: during 1 ~ 1.5:4:1 ~ 1.5; Also below decomposition temperature to 135 DEG C can be reduced.
From table 1,2, the contrast 26 of 3, contrast 27 can find out, when the deal of AC whipping agent is higher, decomposition temperature still higher than 160 DEG C, formamide content higher than 10ppm, the requirement of market to quality product cannot be met; When the deal of AC whipping agent is on the low side, although decomposition temperature, formamide content all meet the requirements, gas forming amount 87mL/g, gas forming amount cannot meet the requirement to product.
From table 1,2, the contrast 24 of 3, contrast 29 can find out, when suppressing the deal of decomposition agent too high, rate of decomposition is down to 0.17mL/ (gmin), and rate of decomposition is too low, affects bubbling efficiency; When suppressing decomposition agent deal too low, rate of decomposition is too fast, causes formamide content higher than 10ppm.
From table 1,2, the contrast 25 of 3 can find out, contrast 25 adopts zinc oxide of the prior art and Zinic stearas as coagent, result: decomposition temperature is higher (being 165 DEG C), formamide content higher (for 240.2ppm) still.
From table 1,2, the contrast 28,30 of 3 can find out, when methane amide remover deal is too low, formamide content is far away higher than 10ppm; When methane amide remover deal is too high, it is a kind of waste of cost.
In specific implementation process, above-mentioned steps (3) preferably adopts micronizer mill to pulverize material, certainly, pulverising step herein also can adopt other grinding mode, such as: mechanical mill etc., but, adopt the pulverizing of micronizer mill fastest, further, be not easy in crushing process to pollute other impurity.
In addition, the pulverising step in above-mentioned steps (2) is preferably and is pulverized to its median size by crushing material is 3 ~ 5 microns, like this, can greatly reduce returning charge rate.
In the present invention used to toluenesulfinic acid zinc, benzene sulfinic acid zinc, tosic acid zinc, ZINC P-PHENOLSULFONATE all purchased from the special fine chemistry industry group of Suzhou City's bass, and be technical pure; Zinc citrate, zinc lactate, Zinic stearas, purchased from Nantong Feiyu Fine Chemicals Co., Ltd., are analytical pure; Trolamine is purchased from the analytical pure of Run Ji chemical industry limited liability company of Xinji City; Tetramethylolmethane is purchased from the technical pure of Kai Linruiyang chemical inc, Jiangsu; Glycerine is purchased from the technical pure of Weifang stars at dawn Chemical Industry Science Co., Ltd; Urotropine is purchased from the technical pure of Guangzhou Gui Hua Chemical Industry Science Co., Ltd; Sodium nitrilo triacetate, nitrilotriacetic acid are all purchased from the technical pure of Shanghai Hui Jin Chemical Co., Ltd.; Sodium ethylene diamine tetracetate is purchased from the technical pure of Baoding Kai Yue Chemical Co., Ltd.; Diethyl malonate is purchased from the technical pure of the sincere company limited in Hebei; Magnesium oxide, magnesium hydroxide, calcium oxide, calcium hydroxide are all purchased from the technical pure of Yingkou XinYao Mei industry company limited.
Claims (8)
1. a low-temperature environment-friendly whipping agent, by AC whipping agent 40 ~ 80 parts, coagent 10 ~ 40 parts, decompose control agent 1 ~ 10 part, methane amide remover 5 ~ 20 parts composition, wherein, coagent is single coagent A or coagent A, B, the mixture of C three, coagent A is to toluenesulfinic acid zinc, benzene sulfinic acid zinc, tosic acid zinc, ZINC P-PHENOLSULFONATE, zinc citrate, zinc lactate, a kind of or several combination in Zinic stearas, coagent B is for using direactive glyceride, stearic acid, in oleic acid any one or severally carry out surface-treated urea or thiocarbamide, coagent C is trolamine, tetramethylolmethane, a kind of or several combination in glycerine, decomposition control agent is a kind of or several combination in hexamethylenetetramine, sodium nitrilo triacetate, nitrilotriacetic acid, sodium ethylene diamine tetracetate, methane amide remover is a kind of or several combination in diethyl malonate, magnesium oxide, magnesium hydroxide, calcium oxide, calcium hydroxide.
2. a kind of low-temperature environment-friendly whipping agent according to claim 1, is characterized in that: the mass ratio of coagent A, B, C is: 1 ~ 1.5:4:1 ~ 1.5.
3. a kind of low-temperature environment-friendly whipping agent according to claim 1, is characterized in that: coagent is 20 ~ 30 parts.
4. a kind of low-temperature environment-friendly whipping agent according to claim 1, is characterized in that: decomposing control agent is 3 ~ 5 parts.
5. according to a kind of low-temperature environment-friendly whipping agent according to claim 1, it is characterized in that: methane amide remover is 5 ~ 8 parts.
6. prepare a method for the low-temperature environment-friendly whipping agent described in any one of claim 1 ~ 5, it is characterized in that, comprise the following steps:
(1) according to the deal of AC whipping agent according to claim 1, coagent, decomposition control agent, methane amide remover, mix;
(2) comminuting matter;
(3) employing 300 ~ 450 orders sieve to remove and do not pulverize coarse particles completely;
(4) fine particle after thick to grinding screen carries out secondary mixing, obtains low-temperature environment-friendly whipping agent product.
7. a kind of method preparing low-temperature environment-friendly whipping agent according to claim 6, is characterized in that: step (3) adopts micronizer mill to pulverize material.
8. a kind of method preparing low-temperature environment-friendly whipping agent according to claim 6, is characterized in that: being pulverized to its median size by crushing material in the pulverising step in step (2) is 3 ~ 5 microns.
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| CN201410104864.8A CN103834055B (en) | 2014-03-20 | 2014-03-20 | A kind of low-temperature environment-friendly whipping agent |
| CN201610390592.1A CN105885078B (en) | 2014-03-20 | 2014-03-20 | The environment-friendly foaming agent of the low formaldehyde of decomposition product and its technique, coagent |
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| CN105504329B (en) * | 2015-12-23 | 2018-11-02 | 江苏索普（集团）有限公司 | The compounding foaming agent and preparation method thereof of expanded material is chemically crosslinked for polyethylene |
| CN105648837A (en) * | 2016-01-04 | 2016-06-08 | 金戈炜业（江苏）壁纸有限公司 | High-foaming coating for printing wallpaper |
| CN105860203A (en) * | 2016-04-26 | 2016-08-17 | 三斯达（江苏）环保科技有限公司 | Environment-friendly safe PE (polyethylene) foamed ground mat and preparation method thereof |
| CN106009026B (en) * | 2016-05-18 | 2018-11-30 | 广州市隆海橡塑有限公司 | A kind of foaming agent, preparation method and application |
| CN110835435B (en) * | 2018-08-16 | 2023-01-13 | 东莞海丽化学材料有限公司 | Formamide absorbent, foaming agent composition and foaming material |
| CN109369949A (en) * | 2018-09-19 | 2019-02-22 | 肇庆凯艺装饰制品有限公司 | A kind of environment-friendly type PS plastic foaming agent |
| CN110734570A (en) * | 2019-09-29 | 2020-01-31 | 浙江杰上杰新材料有限公司 | PVC (polyvinyl chloride) formamide-free foaming agent |
| CN113527768A (en) * | 2021-07-28 | 2021-10-22 | 东莞市智尊新材料科技有限公司 | Degradable environmental-friendly express bag and production equipment thereof |
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| CN101649559B (en) * | 2009-08-31 | 2011-06-22 | 四川大学 | Energy-saving and emission-reduction method for production line of PVC artificial leather |
| CN101824189B (en) * | 2010-04-21 | 2011-11-23 | 北京市射线应用研究中心 | Preparation process of ethylene propylene diene rubber foaming materials |
| CN102432908B (en) * | 2011-08-02 | 2015-06-24 | 杭州海虹精细化工有限公司 | Low-temperature modified foaming agent and preparation method thereof |
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