CN108102530B - Preparation method of flame-retardant polyurea elastomer coating - Google Patents
Preparation method of flame-retardant polyurea elastomer coating Download PDFInfo
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- C08G18/75—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic
- C08G18/751—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring
- C08G18/752—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group
- C08G18/753—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group containing one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group having a primary carbon atom next to the isocyanate or isothiocyanate group
- C08G18/755—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group containing one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group having a primary carbon atom next to the isocyanate or isothiocyanate group and at least one isocyanate or isothiocyanate group linked to a secondary carbon atom of the cycloaliphatic ring, e.g. isophorone diisocyanate
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- C08G18/75—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic
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- C08G18/74—Polyisocyanates or polyisothiocyanates cyclic
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- C08G18/7657—Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings
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Abstract
The invention relates to the technical field of coatings, in particular to a preparation method of a flame-retardant polyurea elastomer coating, which comprises a component A and a component B, and comprises the following steps: (1) uniformly mixing the dehydrated siloxane polyether glycol, diisocyanate and a diluent in a reaction kettle, and then reacting for 2-4 hours at 80-95 ℃ to obtain a component A; (2) and (3) uniformly mixing the dehydrated amine-terminated polyether, the dehydrated amine chain extender, organic aluminum hypophosphite, polytetrafluoroethylene, ammonium polyphosphate, dipentaerythritol and an additive in a reaction kettle, and stirring for 1-2 hours at the temperature of 60-120 ℃ to obtain the component B. According to the invention, the polyurea elastic resin prepared by compounding the flame retardant and the polyurea resin has excellent flame retardance and thermal stability.
Description
Technical Field
The invention relates to the technical field of coatings, in particular to a preparation method of a flame-retardant polyurea elastomer coating.
Background
The spray polyurea elastomer coating is a novel material which does not contain any Volatile Organic Compound (VOC) and has high protection performance and is environment-friendly, and has the advantages of water resistance, corrosion resistance, aging resistance, wear resistance and the like through mixed spray construction.
In the prior art, the flame-retardant polyurea elastomer coating mainly comprises a halogen-containing flame-retardant system and a water-based system. With the enhancement of the awareness of safety and environmental protection of people, the fire-proof performance of many fields such as buildings, traffic, ships and the like is required to be higher. The halogen-free flame retardant has attracted extensive attention due to the characteristics of low toxicity and environmental protection, and non-halogenation is the development trend of the flame retardant in the future. Chinese patent CN201010606500.1 discloses a polyurea intumescent fire-retardant coating, wherein the component A comprises: isocyanate prepolymer, component B comprising: the coating is prepared by burning A, B components into carbon by using a paint film to form a carbonized layer and retard combustion by a combustion mechanism, but because more carbon-forming substances and fillers are added, the viscosity of the component B is not easy to control and is difficult to use and spray. Chinese patent CN201310709700.3 discloses a spray-type flame-retardant antistatic polyurethane elastomer, wherein a component A comprises 40-60 parts of isocyanate and 40-60 parts of phosphorus-containing flame-retardant polyol, and a component B comprises 0-30 parts of chain extender, 0-30 parts of polyether polyol, 10-75 parts of amine-terminated polyether, 0-30 parts of carbon nanotube slurry, 0-3 parts of pigment and 0-3 parts of auxiliary agent.
Disclosure of Invention
The invention aims to provide a preparation method of a flame-retardant polyurea elastomer coating, and the flame-retardant polyurea elastomer coating prepared by the method has excellent flame retardant property and heat resistance.
In order to achieve the above object, the present invention provides a method for preparing a flame retardant polyurea elastomer coating, characterized in that the polyurea elastomer coating comprises a component a and a component B, the method comprising the steps of:
(1) uniformly mixing the dehydrated siloxane polyether glycol, diisocyanate and a diluent in a reaction kettle, and then reacting for 2-4 hours at 80-95 ℃ to obtain a component A;
(2) uniformly mixing the dehydrated amine-terminated polyether, the dehydrated amine chain extender, organic aluminum hypophosphite, polytetrafluoroethylene, ammonium polyphosphate, dipentaerythritol and an additive in a reaction kettle, and stirring at 60-120 ℃ for 1-2 hours to obtain a component B;
(3) mixing the component A and the component B.
Through the technical scheme, the invention has the following technical effects:
the flame retardant is prepared by compounding organic aluminum hypophosphite, polytetrafluoroethylene powder, ammonium polyphosphate and dipentaerythritol, generates a large amount of carbide after combustion, forms a carbonization layer, can extinguish flame in time, can prevent melting and dripping, and has the characteristics of good thermal stability and low smoke generation.
Additional features and advantages of the invention will be set forth in the detailed description which follows.
Detailed Description
The following describes in detail specific embodiments of the present invention. It should be understood that the detailed description and specific examples, while indicating the present invention, are given by way of illustration and explanation only, not limitation.
The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and such ranges or values should be understood to encompass values close to those ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein.
The invention provides a halogen-free flame retardant which comprises organic aluminum hypophosphite, polytetrafluoroethylene, ammonium polyphosphate and dipentaerythritol.
The flame retardant is prepared by compounding organic aluminum hypophosphite, polytetrafluoroethylene powder, ammonium polyphosphate and dipentaerythritol, generates a large amount of carbide after combustion to form a carbonized layer, prevents a matrix from continuing combustion, can prevent melting and dripping, and has the characteristics of good thermal stability and low smoke generation amount.
According to the present invention, in order to optimize the flame retardant performance of the halogen-free flame retardant, under the preferred conditions, the halogen-free flame retardant comprises, based on the total weight of the halogen-free flame retardant being 1: 30-60 wt% of organic aluminum hypophosphite; 3-10 wt% of polytetrafluoroethylene powder; 30-60 wt% of ammonium polyphosphate; 5 to 20 weight percent of dipentaerythritol.
According to the present invention, in order to optimize the flame retardant performance of the halogen-free flame retardant, under the preferred conditions, the halogen-free flame retardant comprises, based on the total weight of the halogen-free flame retardant being 1: 40-50 wt% of organic aluminum hypophosphite; 5-8 wt% of polytetrafluoroethylene powder; 35-43 wt% of ammonium polyphosphate; 10 to 12 weight percent of dipentaerythritol.
The invention also provides a flame-retardant polyurea elastomer coating, which comprises a component A and a component B, wherein the component A is prepared from a raw material composition 1, and the raw material composition 1 comprises: a silicone polyether polyol, a diisocyanate, and optionally a diluent;
the component B is prepared from a raw material composition 2, wherein the raw material composition 2 comprises: amine-terminated polyether, amine chain extender, composite flame retardant and optional additive; the composite flame retardant is the halogen-free flame retardant.
According to the present invention, in order to further optimize the comprehensive properties of the polyurea elastomer coating, the raw material composition 1 preferably comprises, based on the total weight of the component a being 1:
30-50 wt% of siloxane polyether polyol, 45-65 wt% of diisocyanate and 0-5 wt% of diluent.
According to the present invention, under the preferred conditions, the raw material composition 2 comprises, based on the total weight of the component B being 1: 40-60 wt% of amine-terminated polyether, 20-40 wt% of amine chain extender, 10-30 wt% of composite flame retardant and 0-10 wt% of additive.
According to the invention, the flame-retardant polyurea elastomer coating is obtained by mixing the component A and the component B, wherein the weight ratio of the component A to the component B is one of important factors influencing the performance of the flame-retardant polyurea elastomer coating, and under the preferable condition, the weight ratio of the component A to the component B is 1: (0.8 to 1.1).
According to the invention, polyether polyol is one of important raw materials for preparing polyurea elastomer coating, and in order to improve the mechanical property, heat resistance and flame retardance of polyurea, under the preferable conditions, the invention adopts siloxane polyether polyol as the raw material to prepare polyurea elastomer resin, and under the preferable conditions, the siloxane polyether polyol is selected from siloxane polyether diol, and the molecular weight of the siloxane polyether diol is 400-50000.
According to the present invention, preferably, the diisocyanate is at least one selected from the group consisting of 4,4 '-diphenylmethane diisocyanate (4,4' -MDI), 2,4 '-diphenylmethane diisocyanate (2,4' -MDI), Toluene Diisocyanate (TDI), isophorone diisocyanate (IPDI), Hexamethylene Diisocyanate (HDI), and dicyclohexylmethane diisocyanate (HMDI).
According to the present invention, preferably, the diluent is at least one selected from the group consisting of dioctyl phthalate (DOP), butyl phthalate (DBP), propyl carbonate, and ethyl carbonate.
According to the invention, the amino-terminated polyether is preferably selected from polyether diamine and/or polyether triamine, and more preferably at least one of D-230, D-400, T-403, D-2000 and T-5000.
According to the invention, under the preferable conditions, the amine chain extender is at least one selected from MOCA, DEDTA, DADMT, ADA, Unilink4200, Unilink4102, Ethacure100 and Ethacure 300.
According to the present invention, in order to further optimize the properties of the polyurea elastomer coating, it is preferable that the additive includes at least one of a coupling agent, an anti-aging agent, an ultraviolet absorber, an antifoaming agent, and a pigment.
According to the present invention, in order to further optimize the crosslinking degree of the polyurea elastomer coating, it is preferable that the coupling agent is at least one selected from the group consisting of KH550, KH560 and KH 570.
According to the present invention, in order to further optimize the aging resistance of the polyurea elastomer paint, it is preferable that the aging resistance is selected from substituted acrylate-based aging resistance or salicylate-based aging resistance, more specifically, 2-cyano-3, 5-diphenylacrylic acid-ethylhexyl ester; or at least one of phenyl salicylate, benzophenone or benzotriazole compound (BTA).
According to the present invention, in order to further optimize the ultraviolet ray absorption ability of the polyurea elastomer coating, it is preferable that the ultraviolet ray absorber is at least one selected from the group consisting of UV-9, UV-329 and UV-328.
According to the invention, the defoaming agent is preferably at least one selected from BYK085, BYK410 and BYK 425.
According to the invention, in order to improve the aesthetic degree of the polyurea elastomer coating, the polyurea elastomer coating also contains pigment, the type of the pigment has no special requirement, and can be adjusted according to practical application, and under the preferable condition, the pigment is selected from at least one of titanium dioxide, phthalocyanine blue, phthalocyanine green and high-pigment carbon black.
The invention also provides a preparation method of the polyurea elastomer coating, which comprises the following steps:
(1) uniformly mixing the dehydrated siloxane polyether glycol, diisocyanate and a diluent in a reaction kettle, and then reacting for 2-4 hours at 80-95 ℃ to obtain a component A;
(2) and (3) uniformly mixing the dehydrated amine-terminated polyether, the dehydrated amine chain extender, organic aluminum hypophosphite, polytetrafluoroethylene, ammonium polyphosphate, dipentaerythritol and an additive in a reaction kettle, and stirring for 1-2 hours at the temperature of 60-120 ℃ to obtain the component B.
According to the invention, in order to optimize the reaction efficiency, the raw materials are subjected to reduced pressure dehydration before the reaction, and the dehydration process of the siloxane polyether glycol is as follows under the preferable conditions: the temperature is 100-120 ℃, the pressure is 0.02-0.1 MPa, and the time is 1-3 h.
According to the invention, in order to optimize the reaction efficiency, before the reaction, the raw materials are subjected to reduced pressure dehydration, and under the preferable conditions, the dehydration process of the amine chain extender comprises the following steps: the temperature is 100-120 ℃, the pressure is 0.02-0.1 MPa, and the time is 1-3 h.
According to the invention, in order to optimize the reaction efficiency, the raw materials are subjected to reduced pressure dehydration before the reaction, and the dehydration process of the amino-terminated polyether comprises the following steps under the preferable conditions: the temperature is 100-120 ℃, the pressure is 0.02-0.1 MPa, and the time is 1-3 h.
The present invention will be described in detail below by way of examples.
In the following examples, silicone polyether glycol (Wacker IM 22) was purchased from Wacker-Chemie-GmbH and had a molecular weight of 400-50000; 4,4' -MDI, HDI, HMDI, IPDI are available from Wanhua chemical group GmbH, TDI is available from Corsai, DOP, DBP are available from Shandong Kanghua chemical Co., Ltd, propyl carbonate is available from Jiangsu Fengming chemical technology Co., Ltd, D-2000, D-230, T-403, T-5000 is available from Hunsmei, Ethacure300 is available from Yabao in USA, Unilink4200 is available from Dorf Ketal, MoCA, DADMT, DEDTA is available from Suzhou Xiangyuan chemical Co., Ltd, organic aluminum hypophosphite, polytetrafluoroethylene powder, ammonium polyphosphate, dipentaerythritol is available from Shenjinhang Kanglong chemical technology Co., Ltd, KH560, KH570 is available from Dow Corning, BTA, UV-329, UV-328 is available from Pasteur, BYK085, BYK410 is available from BYK, titanium dioxide is available from DuPont.
Example 1
The contents of the respective raw materials in component A and component B in this example are shown in Table 1.
(1) Dehydrating 40 parts by weight of silicone polyether glycol for 2 hours at the temperature of 110 ℃ and the pressure of 0.05MPa, uniformly mixing the dehydrated silicone polyether glycol with 55 parts by weight of 4,4' -MDI and 5 parts by weight of DOP in a reaction kettle, and then reacting for 3 hours at the temperature of 90 ℃ to obtain a component A;
(2) 50 parts by weight of D-2000 and 30 parts by weight of Ethacure300 are respectively dehydrated for 1.5 hours under the conditions that the temperature is 110 ℃ and the pressure is 0.05MPa, and then the dehydrated D-2000 and the dehydrated Ethacure300 are uniformly mixed with 8 parts by weight of organic aluminum hypophosphite, 1 part by weight of polytetrafluoroethylene, 8 parts by weight of ammonium polyphosphate and 3 parts by weight of dipentaerythritol in a reaction kettle, and the mixture is stirred for 1.5 hours at 90 ℃ to obtain a component B.
Table 1: example 1 content of each raw Material in component A and component B
Example 2
The contents of the respective raw materials in component A and component B in this example are shown in Table 2.
(1) 50 parts by weight of siloxane polyether dihydric alcohol is dehydrated for 2 hours under the conditions that the temperature is 110 ℃ and the pressure is 0.02MPa, then the dehydrated siloxane polyether dihydric alcohol is uniformly mixed with 45 parts by weight of 4,4' -MDI and 5 parts by weight of DBP in a reaction kettle, and then the mixture is reacted for 3 hours at 85 ℃ to obtain a component A;
(2) 50 parts by weight of D-2000 and 30 parts by weight of Unilink4200 are dehydrated for 2 hours under the conditions that the temperature is 110 ℃ and the pressure is 0.05MPa respectively, and then the dehydrated D-2000 and the dehydrated Unilink4200 are uniformly mixed with 6 parts by weight of organic aluminum hypophosphite, 1 part by weight of polytetrafluoroethylene, 12 parts by weight of ammonium polyphosphate and 1 part by weight of dipentaerythritol in a reaction kettle, and the mixture is stirred for 1 hour at the temperature of 100 ℃ to obtain the component B.
Table 2: example 2 content of each raw Material in component A and component B
Example 3
The contents of the respective raw materials in component A and component B in this example are shown in Table 3.
(1) Dehydrating 35 parts by weight of silicone polyether glycol for 1 hour at the temperature of 120 ℃ and the pressure of 0.1MPa, uniformly mixing the dehydrated silicone polyether glycol and 65 parts by weight of TDI in a reaction kettle, and reacting for 2 hours at the temperature of 95 ℃ to obtain a component A;
(2) 30 parts by weight of D-230 and 40 parts by weight of Ethacure300 are dehydrated for 1.5 hours under the conditions that the temperature is 120 ℃ and the pressure is 0.1MPa, and then the dehydrated D-230 and the dehydrated Ethacure300 are uniformly mixed with 9 parts by weight of organic aluminum hypophosphite, 1.5 parts by weight of polytetrafluoroethylene, 16.5 parts by weight of ammonium polyphosphate and 3 parts by weight of dipentaerythritol in a reaction kettle, and the mixture is stirred for 1.5 hours at the temperature of 80 ℃ to obtain the component B.
Table 3: example 3 content of each raw Material in component A and component B
Example 4
The contents of the respective raw materials in component A and component B in this example are shown in Table 4.
(1) 50 parts by weight of silicone polyether glycol is dehydrated for 1.5h at the temperature of 120 ℃ and the pressure of 0.02MPa, then the dehydrated silicone polyether glycol is uniformly mixed with 45 parts by weight of HDI and 5 parts by weight of DOP in a reaction kettle, and then the mixture reacts for 4h at the temperature of 95 ℃ to obtain a component A;
(2) 60 parts by weight of T-403 and 29 parts by weight of Unilink4200 are dehydrated for 3 hours at a temperature of 120 ℃ and a pressure of 0.02MPa, and then the dehydrated T-403 and Unilink4200 are uniformly mixed with 6 parts by weight of aluminum organophosphite, 0.5 part by weight of polytetrafluoroethylene, 3 parts by weight of ammonium polyphosphate, 0.5 part by weight of dipentaerythritol and 1 part by weight of KH560 in a reaction kettle, and stirred for 2 hours at a temperature of 60 ℃ to obtain component B.
Table 4: example 4 content of each raw Material in component A and component B
Example 5
The contents of the respective raw materials in component A and component B in this example are shown in Table 5.
(1) Dehydrating 30 parts by weight of siloxane polyether glycol for 3 hours at the temperature of 100 ℃ and the pressure of 0.1MPa, uniformly mixing the dehydrated siloxane polyether glycol, 65 parts by weight of HDI and 5 parts by weight of DBP in a reaction kettle, and reacting for 2 hours at the temperature of 80 ℃ to obtain a component A;
(2) dehydrating 60 parts by weight of T-403 and 20 parts by weight of MoCA for 1 hour at the temperature of 120 ℃ and under the pressure of 0.02MPa, uniformly mixing the dehydrated T-403 and MoCA with 4.5 parts by weight of organic aluminum hypophosphite, 1.5 parts by weight of polytetrafluoroethylene, 6 parts by weight of ammonium polyphosphate, 3 parts by weight of dipentaerythritol, 1 part by weight of titanium dioxide, 1 part by weight of BYK085, 1 part by weight of UV-329, 1 part by weight of BTA and 1 part by weight of KH560 in a reaction kettle, and stirring for 1 hour at the temperature of 120 ℃ to obtain the component B.
Table 5: example 5 content of each raw Material in component A and component B
Example 6
In this example, the preparation method of the flame-retardant polyurea elastomer coating is the same as that in example 1, except that the content ratio of each substance is different, and the content of each raw material in the component a and the component B in this example is shown in table 6.
Table 6: example 6 content of each raw Material in component A and component B
Example 7
In this example, the preparation method of the flame-retardant polyurea elastomer coating is the same as that in example 1, except that the content ratio of each substance is different, and the content of each raw material in the component a and the component B in this example is shown in table 7.
Table 7: example 7 content of each raw Material in component A and component B
Example 8
In this example, the preparation method of the flame-retardant polyurea elastomer coating is the same as that in example 1, except that the content ratio of each substance is different, and the content of each raw material in the component a and the component B in this example is shown in table 8.
Table 8: example 8 content of each raw Material in component A and component B
Example 9
In this example, the preparation method of the flame-retardant polyurea elastomer coating is the same as that in example 1, except that the content ratio of each substance is different, and the content of each raw material in the component a and the component B in this example is shown in table 9.
Table 9: example 9 content of each raw Material in component A and component B
Comparative example 1
The process of example 1 was followed except that the flame retardant did not contain an organic aluminum hypophosphite.
Comparative example 2
The procedure of example 1 was followed except that the flame retardant did not contain polytetrafluoroethylene powder.
Comparative example 3
The process of example 1 was followed except that the flame retardant did not contain ammonium polyphosphate.
Comparative example 4
The process of example 1 was followed except that dipentaerythritol was not included in the flame retardant.
Comparative example 5
The procedure of example 1 was followed except that polyoxypropylene diol was used in place of the silicone polyether diol.
The construction method comprises the following steps:
the A, B two components are used according to the volume ratio of 1:1, sprayed onto a substrate through a spray gun, and cured to obtain the polyurea elastomer material, wherein the pressure of a spraying machine is set to be 2400psi, the temperature is set to be 60 ℃, the spraying pressure difference of the two components in a spray gun mixing chamber is lower than 400psi, and the polyurea elastomer sprayed and formed into a film is cured for seven days under constant temperature and humidity.
The test method comprises the following steps: the flame retardant properties of the polyurea elastic coatings of examples 1 to 9 and comparative examples 1 to 5 were tested according to the methods of GBT 2406-.
Table 10: performance Table of polyurea elastic coating materials in examples 1 to 9 and comparative examples 1 to 5
The preferred embodiments of the present invention have been described in detail, however, the present invention is not limited to the specific details of the above embodiments, and various simple modifications may be made to the technical solution of the present invention within the technical idea of the present invention, and these simple modifications are within the protective scope of the present invention.
It should be noted that the various technical features described in the above embodiments can be combined in any suitable manner without contradiction, and the invention is not described in any way for the possible combinations in order to avoid unnecessary repetition.
In addition, any combination of the various embodiments of the present invention is also possible, and the same should be considered as the disclosure of the present invention as long as it does not depart from the spirit of the present invention.
Claims (7)
1. The preparation method of the flame-retardant polyurea elastomer coating is characterized by comprising the following steps:
(1) uniformly mixing the dehydrated siloxane polyether glycol, diisocyanate and a diluent in a reaction kettle, and then reacting for 2-4 hours at 80-95 ℃ to obtain a component A;
(2) uniformly mixing the dehydrated amine-terminated polyether, the dehydrated amine chain extender, organic aluminum hypophosphite, polytetrafluoroethylene, ammonium polyphosphate, dipentaerythritol and an additive in a reaction kettle, and stirring at 60-120 ℃ for 1-2 hours to obtain a component B;
(3) mixing the component A and the component B;
wherein the molecular weight of the silicone polyether glycol is 400-50000.
2. The preparation method of claim 1, wherein the dehydration processes of the silicone polyether glycol, the amino terminated polyether and the amine chain extender are each independently: the temperature is 100-120 ℃, the pressure is 0.02-0.1 MPa, and the time is 1-3 h.
3. The production method according to claim 1, wherein the diisocyanate is one selected from the group consisting of 4,4 '-diphenylmethane diisocyanate, 2,4' -diphenylmethane diisocyanate, tolylene diisocyanate, isophorone diisocyanate, hexamethylene diisocyanate, and dicyclohexylmethane diisocyanate.
4. The production method according to claim 1, wherein the diluent is selected from at least one of dioctyl phthalate, butyl phthalate, propyl carbonate, and ethyl carbonate.
5. The method of claim 1, wherein the amine-terminated polyether is selected from polyether diamine and/or polyether triamine.
6. The production method according to claim 1, wherein the amine chain extender is at least one selected from MOCA, DEDTA, dmt, ADA, Unilink4200, Unilink4102, Ethacure100, and Ethacure 300.
7. The production method according to any one of claim 1, wherein the additive includes at least one of a coupling agent, an age resistor, an ultraviolet absorber, an antifoaming agent, and a pigment.
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CN107141591A (en) * | 2017-06-08 | 2017-09-08 | 北京化工大学 | A kind of few additive halogen-free anti-flaming polypropylene material and preparation method thereof |
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