CN114591569B - Preparation method of flame-retardant filler, composite material containing flame-retardant filler and preparation method of composite material - Google Patents
Preparation method of flame-retardant filler, composite material containing flame-retardant filler and preparation method of composite material Download PDFInfo
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- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
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- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
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- C08L67/00—Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
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- C08L77/00—Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
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- C08K2003/2224—Magnesium hydroxide
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Abstract
The invention discloses a preparation method of a flame-retardant filler, a composite material containing the flame-retardant filler and a preparation method thereof, wherein the preparation method of the flame-retardant material comprises the following steps: (1) Boehmite, chitosan, acetic acid, glyoxal and deionized water are put into a reaction vessel to react to obtain a solution A; (2) Putting the solution A, magnesium nitrate and ammonia water into a reaction vessel for reaction to obtain a solution B; (3) And (3) carrying out suction filtration, washing and drying on the solution B to obtain the boehmite/chitosan/magnesium hydroxide type flame-retardant filler. Under the synergistic effect of boehmite, chitosan and magnesium hydroxide, the carbon residue generated by polyolefin in the combustion process is anchored on the framework of the boehmite, so that the stability of the framework of the boehmite is enhanced, and continuous and compact carbon residue is formed; magnesium hydroxide can generate magnesium oxide when heated, and the existence of the magnesium oxide promotes the formation of a carbon layer with higher hardness, so that the resistance of the carbon layer to heat and gas is enhanced, and the release of heat and toxic smoke is reduced.
Description
Technical Field
The invention relates to the technical field of flame retardants, in particular to a preparation method of a flame retardant filler, a composite material containing the flame retardant filler and a preparation method of the composite material.
Background
The flame retardant property is one of important properties of automobile interior and exterior decorative parts, plastic shells and the like, and a plurality of methods for improving the flame retardant property of the polymer exist. Polyolefin is mainly composed of carbon, ammonia and oxygen atoms, so polyolefin is generally inflammable, and there are many methods for improving flame retardant properties of polyolefin, but conventional methods are to add flame retardant filler into polyolefin. The existing flame-retardant filler is a conventional filler, and has poor compatibility with polyolefin when being mixed.
The flame-retardant filler prepared by the invention improves the flame retardant property of the prior polyolefin, and the flame-retardant composite filler has not been reported yet.
Disclosure of Invention
The invention aims to solve the technical problem of providing a preparation method of flame-retardant filler, a composite material containing the flame-retardant filler and a preparation method thereof, and the flame-retardant filler can improve the flame-retardant property of the existing polyolefin.
The technical problems to be solved by the invention are realized by the following technical scheme:
a method for preparing a flame retardant filler, comprising the steps of:
(1) Boehmite, chitosan, acetic acid, glyoxal and deionized water are put into a reaction vessel to react for 6-8 hours at the temperature of 60-80 ℃ to obtain solution A;
(2) Placing the solution A, magnesium nitrate and ammonia water into a reaction vessel for reaction for 8-10 hours at 50-70 ℃ to obtain a solution B;
(3) And (3) carrying out suction filtration, washing and drying on the solution B to obtain the boehmite/chitosan/magnesium hydroxide type flame-retardant filler.
Preferably, in the above technical scheme, the mass ratio of boehmite, chitosan, acetic acid, glyoxal and deionized water in the step (1) is (30-40): (20-30): (60-80): (18-24): (50-70).
Preferably, in the above technical scheme, the mass ratio of the solution a, magnesium nitrate and ammonia water in the step (2) is (60-80): (20-30): (18-20).
Preferably, in the above technical solution, the reaction conditions in the reaction vessel in step (1) are: reacting for 7h at 70 ℃; the reaction conditions in the reaction vessel in the step (2) are as follows: the reaction was carried out at 60℃for 9h.
The flame-retardant filler is prepared by a preparation method of the flame-retardant filler.
The composite material comprises the following components in parts by weight: polyolefin material 80 and flame retardant material 20, the flame retardant material being prepared according to a method of preparing the flame retardant material.
Preferably, in the above technical solution, the thermoplastic is Polyethylene (PE), polypropylene (PP), polystyrene (PS), polybutylene terephthalate (PBT) or polyamide 6 (PA 6).
A method of preparing a composite material comprising the steps of:
and mixing the flame retardant material and the polyolefin material according to parts by weight, stirring for 10min by a high-speed mixer, and adding into a double-screw extruder for blending extrusion to obtain the composite material.
Preferably, in the above technical scheme, the twin-screw extruder comprises six temperature areas which are sequentially arranged, wherein the temperature of the first temperature area is 120-230 ℃, the temperature of the second temperature area is 180-260 ℃, the temperature of the third temperature area is 180-260 ℃, the temperature of the fourth temperature area is 180-260 ℃, the temperature of the fifth temperature area is 180-260 ℃, the temperature of the sixth temperature area is 180-260 ℃, the temperature of the head of the twin-screw extruder is 180-260 ℃, and the screw rotating speed is 200-320r/min.
The technical scheme of the invention has the following beneficial effects:
(1) The preparation method comprises the steps of firstly utilizing an aldol condensation reaction mechanism of glyoxal and chitosan to finish the surface adsorption of chitosan on boehmite, then utilizing magnesium nitrate to react with ammonia water to generate magnesium hydroxide, and finally preparing the boehmite/chitosan/magnesium hydroxide type flame retardant filler.
(2) Boehmite can generate water and Al in the process of thermal decomposition 2 O 3 The water can dilute the combustible gas, al 2 O 3 The solid is covered on the surface of the polyolefin matrix to block and delay the burning rate, thereby achieving the effects of flame retardance and smoke suppression.
(3) Under the synergistic effect of boehmite, chitosan and magnesium hydroxide, the carbon residue generated by polyolefin in the combustion process is anchored on the framework of the boehmite, so that the stability of the framework of the boehmite is enhanced, and continuous and compact carbon residue is formed. Magnesium hydroxide can generate magnesium oxide when heated, and the existence of the magnesium oxide promotes the formation of a carbon layer with higher hardness, so that the resistance of the carbon layer to heat and gas is enhanced, and the release of heat and toxic smoke is reduced.
Detailed Description
Various exemplary embodiments of the invention will now be described in detail. It should be noted that: the relative arrangement of the components and steps, numerical expressions and numerical values set forth in these embodiments do not limit the scope of the present invention unless it is specifically stated otherwise.
The raw materials used in the examples of the present invention are as follows:
PBT (model 2002U), japanese Bao Ji; PP (model Z30S), luxuriant petrochemical; PE (model 5070), panjin ethylene; PA6 (model CM 1017), eastern japan; PS (model 350), taiwan arbor; boehmite, zibo Jin Qi chemical technology Co., ltd; chitosan, shanghai Yi En chemical technologies limited; acetic acid, su state warfarin chemical technology limited; adipaldehyde, hubei Xinrun chemical Co., ltd; magnesium nitrate, nanjing fine noro chemical technology Co., ltd; ammonia, atanan Meng Qiao chemical company, inc; deionized water, xiamen Australia Environment protection technology Co.
The test instrument used in the invention is as follows:
a ZSK30 twin-screw extruder, W & P, germany; an internal mixer, a large Lian Huahan rubber plastic; JL-1000 tensile tester, produced by Guangzhou Guangdong talent laboratory instruments; HTL900-T-5B injection molding machine, produced by Heterol plastics machinery Co., ltd; XCJ-500 impact tester, manufactured by the underwriter's tester; QT-1196 tensile tester, toguan, gaotai detection instruments, inc.; QD-GJS-B12K high-speed mixer, beijing Hengaode instruments and meters Co.
Example 1
Preparation example 1
A method for preparing a flame retardant filler, comprising the steps of:
(1) 300g of boehmite, 200g of chitosan, 600g of acetic acid, 180g of glyoxal and 500g of deionized water are weighed and put into a reaction vessel to react for 6 hours at 60 ℃ to obtain solution A.
(2) 600g of solution A, 200g of magnesium nitrate and 180g of ammonia water are weighed and put into a reaction vessel to react for 8 hours at 50 ℃ to obtain solution B.
(3) And carrying out suction filtration, washing and drying on the solution B to obtain the boehmite/chitosan/magnesium hydroxide type flame retardant filler P1.
Application example 1
A method of preparing a composite material comprising the steps of:
20 parts of P1 are added into 80 Parts of Polypropylene (PP), stirred for 10min by a high-speed mixer, and then added into a double-screw extruder for blending extrusion, so as to obtain the PP composite material X1.
The twin-screw extruder comprises six temperature areas which are sequentially arranged, wherein the temperature of the first temperature area is 170 ℃, the temperature of the second temperature area is 220 ℃, the temperature of the third temperature area is 230 ℃, the temperature of the fourth temperature area is 240 ℃, the temperature of the fifth temperature area is 240 ℃, the temperature of the sixth temperature area is 240 ℃, the temperature of the head of the twin-screw extruder is 230 ℃, and the screw rotating speed is 220r/min.
Comparative example 1
80 Parts of Polypropylene (PP) is taken and stirred for 10min by a high-speed mixer, and then added into a double-screw extruder for blending extrusion, so as to obtain the PP composite material D1.
The performance data of the PP composite materials prepared in the above application example 1 and comparative example 1 are shown in the following table (table 1):
TABLE 1
As can be seen from the above table, the flame retardant property of X1 is better than that of D1, which indicates that the flame retardant property of PP is better after the flame retardant filler of the invention is added.
Example 2
Preparation example 2
A method for preparing a flame retardant filler, comprising the steps of:
(1) 350g of boehmite, 250g of chitosan, 700g of acetic acid, 210g of glyoxal and 600g of deionized water are weighed and put into a reaction vessel to react for 7 hours at 70 ℃ to obtain solution A.
(2) 700g of solution A, 250g of magnesium nitrate and 190g of ammonia water are weighed and put into a reaction vessel to react for 9 hours at 60 ℃ to obtain solution B.
(3) And carrying out suction filtration, washing and drying on the solution B to obtain the boehmite/chitosan/magnesium hydroxide type flame retardant filler P2.
Application example 2
A method of preparing a composite material comprising the steps of:
20 parts of P2 are added into 80 parts of polybutylene terephthalate (PBT), stirred for 10min by a high-speed mixer, and then added into a double-screw extruder for blending extrusion, so as to obtain the PBT composite material X2.
The twin-screw extruder comprises six temperature areas which are sequentially arranged, wherein the temperature of the first temperature area is 200 ℃, the temperature of the second temperature area is 260 ℃, the temperature of the third temperature area is 260 ℃, the temperature of the fourth temperature area is 260 ℃, the temperature of the fifth temperature area is 260 ℃, the temperature of the sixth temperature area is 260 ℃, the temperature of the head of the twin-screw extruder is 260 ℃, and the screw rotating speed is 300r/min.
Comparative example 2
80 parts of PBT is taken, stirred for 10min by a high-speed mixer, and then added into a double-screw extruder for blending extrusion, so as to obtain the PBT composite material D2.
The performance data of the PBT composite materials prepared in the application example 2 and the comparative example 2 are shown in the following table (Table 2):
TABLE 2
As can be seen from the above table, the flame retardant properties of X2 are better than those of D2, which indicates that the flame retardant properties of PBT are better after the flame retardant filler of the invention is added.
Example 3
Preparation example 3
A method for preparing a flame retardant filler, comprising the steps of:
(1) 400g of boehmite, 300g of chitosan, 800g of acetic acid, 240g of glyoxal and 700g of deionized water are weighed and put into a reaction vessel to react for 8 hours at 80 ℃ to obtain solution A.
(2) 800g of solution A, 300g of magnesium nitrate and 200g of ammonia water are weighed and put into a reaction vessel to react for 10 hours at 70 ℃ to obtain solution B.
(3) And carrying out suction filtration, washing and drying on the solution B to obtain the boehmite/chitosan/magnesium hydroxide type flame retardant filler P3.
Application example 3
A method of preparing a composite material comprising the steps of:
20 parts of P3 are added into 80 parts of Polyethylene (PE), stirred for 10min by a high-speed mixer, and then added into a double-screw extruder for blending extrusion, so as to obtain PE composite material X3.
The twin-screw extruder comprises six temperature areas which are sequentially arranged, wherein the temperature of the first temperature area is 120 ℃, the temperature of the second temperature area is 180 ℃, the temperature of the third temperature area is 180 ℃, the temperature of the fourth temperature area is 180 ℃, the temperature of the fifth temperature area is 180 ℃, the temperature of the sixth temperature area is 180 ℃, the temperature of the head of the twin-screw extruder is 180 ℃, and the screw rotating speed is 300r/min.
Comparative example 3
Taking 80 parts of PE, stirring for 10min by a high-speed mixer, and then adding the PE into a double-screw extruder for blending extrusion to obtain the PE composite material D3.
The performance data of the PE composite materials prepared in the above application example 3 and comparative example 3 are shown in the following table (table 3):
TABLE 3 Table 3
As can be seen from the above table, the flame retardant property of X3 is better than that of D3, which indicates that the flame retardant property of PE is better after the flame retardant filler is added.
Example 4
Preparation example 4
A method for preparing a flame retardant filler, comprising the steps of:
(1) 385g of boehmite, 275g of chitosan, 655g of acetic acid, 215g of glyoxal and 550g of deionized water are weighed and put into a reaction vessel for reaction for 7 hours at 650 ℃ to obtain a solution A.
(2) 625g of solution A, 245g of magnesium nitrate and 195g of ammonia water are weighed and put into a reaction vessel for reaction for 9 hours at 55 ℃ to obtain solution B.
(3) And carrying out suction filtration, washing and drying on the solution B to obtain the boehmite/chitosan/magnesium hydroxide type flame retardant filler P4.
Application example 4
A method of preparing a composite material comprising the steps of:
20 parts of P4 are added into 80 parts of polyamide 6 (PA 6), stirred for 10min by a high-speed mixer, and then added into a double-screw extruder for blending extrusion, so as to obtain the PA6 composite material X4.
The twin-screw extruder comprises six temperature areas which are sequentially arranged, wherein the temperature of the first temperature area is 230 ℃, the temperature of the second temperature area is 260 ℃, the temperature of the third temperature area is 260 ℃, the temperature of the fourth temperature area is 260 ℃, the temperature of the fifth temperature area is 260 ℃, the temperature of the sixth temperature area is 260 ℃, the temperature of the head of the twin-screw extruder is 250 ℃, and the screw rotating speed is 320r/min.
Comparative example 4
Taking 80 parts of PA6, stirring for 10min by a high-speed mixer, and then adding into a double-screw extruder for blending extrusion to obtain the PA6 composite material D4.
The performance data of the PA6 composite materials prepared in the above application example 4 and comparative example 4 are shown in the following table (table 4):
TABLE 4 Table 4
As can be seen from the above table, the flame retardant properties of X4 are better than those of D4, which indicates that the flame retardant properties of PA6 are better after the flame retardant filler of the invention is added.
Example 5
Preparation example 5
A method for preparing a flame retardant filler, comprising the steps of:
(1) 315g of boehmite, 285g of chitosan, 665g of acetic acid, 195g of glyoxal and 625g of deionized water are weighed and put into a reaction vessel for reaction for 7 hours at 75 ℃ to obtain a solution A.
(2) 715g of solution A, 235g of magnesium nitrate and 195g of ammonia water are weighed and put into a reaction vessel for reaction for 8 hours at 65 ℃ to obtain solution B.
(3) And carrying out suction filtration, washing and drying on the solution B to obtain the boehmite/chitosan/magnesium hydroxide type flame retardant filler P5.
Application example 5
A method of preparing a composite material comprising the steps of:
20 parts of P5 are added into 80 Parts of Styrene (PS), stirred for 10min by a high-speed mixer, and then added into a double-screw extruder for blending extrusion, so as to obtain the PS composite material X5.
The twin-screw extruder comprises six temperature areas which are sequentially arranged, wherein the temperature of the first temperature area is 160 ℃, the temperature of the second temperature area is 200 ℃, the temperature of the third temperature area is 200 ℃, the temperature of the fourth temperature area is 200 ℃, the temperature of the fifth temperature area is 200 ℃, the temperature of the sixth temperature area is 200 ℃, the temperature of the head of the twin-screw extruder is 200 ℃, and the screw rotating speed is 280r/min.
Comparative example 5
80 parts of PS is taken and stirred for 10min by a high-speed mixer, and then added into a double-screw extruder for blending extrusion, so that the PS composite material D5 is obtained.
The performance data of PS composite materials prepared in the above application example 5 and comparative example 5 are shown in the following table (table 5):
TABLE 5
As can be seen from the above table, the flame retardant properties of X5 are better than those of D5, which indicates that the flame retardant properties of PS are better after the flame retardant filler of the invention is added.
The flame-retardant filler and the preparation method thereof have the advantages that the flame-retardant performance of the polyolefin material prepared by the flame-retardant filler is improved to a great extent, and the flame-retardant filler has very important significance.
Although the present invention has been described with reference to the above embodiments, it should be understood that the present invention is not limited thereto, and that various changes and modifications may be made by those skilled in the art without departing from the spirit and scope of the present invention, and the scope of the present invention is defined by the appended claims and their equivalents.
Claims (8)
1. A method for preparing a flame retardant filler, comprising the steps of:
(1) Boehmite, chitosan, acetic acid, glyoxal and deionized water are put into a reaction vessel to react for 6-8 hours at the temperature of 60-80 ℃ to obtain solution A;
(2) Placing the solution A, magnesium nitrate and ammonia water into a reaction vessel for reaction for 8-10 hours at 50-70 ℃ to obtain a solution B;
(3) And (3) carrying out suction filtration, washing and drying on the solution B to obtain the boehmite/chitosan/magnesium hydroxide type flame-retardant filler.
2. The method for preparing the flame-retardant filler according to claim 1, wherein the mass ratio of boehmite, chitosan, acetic acid, glyoxal and deionized water in the step (1) is (30-40): (20-30): (60-80): (18-24): (50-70).
3. The method for preparing the flame-retardant filler according to claim 1, wherein the mass ratio of the solution a, magnesium nitrate and ammonia water in the step (2) is (60-80): (20-30): (18-20).
4. The method for producing a flame retardant filler according to claim 1, wherein the reaction conditions in the reaction vessel in step (1) are: reacting for 7h at 70 ℃; the reaction conditions in the reaction vessel in the step (2) are as follows: the reaction was carried out at 60℃for 9h.
5. A flame retardant filler, characterized in that it is prepared by the method for preparing a flame retardant filler according to any one of claims 1 to 4.
6. The composite material is characterized by comprising the following components in parts by weight: a polyolefin material 80 and a flame retardant material 20, the flame retardant material being prepared according to the method for preparing a flame retardant filler according to any one of claims 1 to 4.
7. The method of preparing a composite material according to claim 6, comprising the steps of:
and mixing the flame retardant material and the polyolefin material according to parts by weight, stirring for 10min by a high-speed mixer, and adding into a double-screw extruder for blending extrusion to obtain the composite material.
8. The method of producing a composite material according to claim 7, wherein the twin-screw extruder comprises six temperature zones arranged in sequence, the temperature of the first temperature zone is 120-230 ℃, the temperature of the second temperature zone is 180-260 ℃, the temperature of the third temperature zone is 180-260 ℃, the temperature of the fourth temperature zone is 180-260 ℃, the temperature of the fifth temperature zone is 180-260 ℃, the temperature of the sixth temperature zone is 180-260 ℃, the temperature of the head of the twin-screw extruder is 180-260 ℃, and the screw rotation speed is 200-320r/min.
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| CN202210345723.XA CN114591569B (en) | 2022-03-31 | 2022-03-31 | Preparation method of flame-retardant filler, composite material containing flame-retardant filler and preparation method of composite material |
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| FR2967997B1 (en) * | 2010-11-26 | 2017-12-22 | Saint-Gobain Technical Fabrics Europe | FLAME RETARDANT COMPOSITION BASED ON MINERAL FIBERS, AND MATS OBTAINED. |
| JP2017082163A (en) * | 2015-10-30 | 2017-05-18 | 神島化学工業株式会社 | Composite additive containing magnesium hydroxide particle |
| CN109320775A (en) * | 2018-09-20 | 2019-02-12 | 安徽江淮汽车集团股份有限公司 | A kind of preparation method of the fire-retardant compounded mix of low VOC |
| CN110343383B (en) * | 2019-06-12 | 2022-04-01 | 浙江新力新材料股份有限公司 | Boehmite-magnesium hydroxide synergistic flame-retardant nylon composite material and preparation method and application thereof |
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