A method for preparing fire-resistant and flame-retardant PVC material

Abstract

The invention belongs to the technical field of PVC materials, and is specifically a method for preparing a fire-resistant and flame-retardant PVC material. The method comprises the following specific steps: using laser drilling to punch a plurality of micropores on PVC particles, then immersing the PVC particles in a flame-retardant solution, and after the immersion is complete, taking out the PVC particles to form a flame-retardant layer on the PVC particles. The invention adds decabromodiphenyl ether, tetrabromobisphenol A, decabromodiphenyl ethane and tetrabromoether to raw materials, and forms a flame-retardant layer on the inner and outer surfaces of the PVC particles, thereby greatly improving the fire-resistant and flame-retardant performance of the PVC material, so as to avoid the phenomenon of continuous combustion of the PVC material due to long-term combustion to a certain extent, thereby improving safety.

Description

Technical Field

[0001] The invention relates to the technical field of PVC materials, in particular to a method for preparing a fire-resistant and flame-retardant PVC material. Background Art

[0002] PVC material (polyvinyl chloride) is a high molecular polymer produced by free radical polymerization of vinyl chloride monomer. It is the third largest synthetic polymer plastic in the world, second only to polyethylene and polypropylene. PVC material has two types: hard and soft. Hard PVC is mainly used for building pipes, doors and windows, etc., while soft PVC can be made soft and elastic by adding plasticizers, and is suitable for cable insulation, flooring, signs and other purposes.

[0003] However, the existing PVC material has certain limitations in its fire-resistant and flame-retardant properties. It will continue to burn when burned for a long time, which will cause certain safety hazards. Therefore, a method for preparing a fire-resistant and flame-retardant PVC material is invented. Summary of the invention

[0004] To solve the above technical problems, according to one aspect of the present invention, the present invention provides the following technical solutions: A method for preparing a fire-resistant and flame-retardant PVC material comprises the following specific steps: Step 1, preparation of raw materials: polyvinyl chloride, calcium stearate, acrylate, paraffin, polypropylene, composite stabilizer, plasticizer, coupling agent, antioxidant, enhancer, preservative, decabromodiphenyl ether, tetrabromobisphenol A, decabromodiphenyl ethane, tetrabromoether; Step 2, grinding: grinding polyvinyl chloride, calcium stearate, acrylate, paraffin, polypropylene, composite stabilizer, coupling agent, antioxidant, reinforcing agent, preservative, decabromodiphenyl ether, tetrabromobisphenol A, decabromodiphenyl ethane and tetrabromoether to obtain a powdery material; Step 3, mixing: first, polyvinyl chloride, calcium stearate, acrylate, paraffin and polypropylene are mixed for 10 min-16 min to obtain mixture A, then, the composite stabilizer, coupling agent, antioxidant, reinforcing agent and preservative are mixed for 10 min-16 min to obtain mixture B, then, decabromodiphenyl ether, tetrabromobisphenol A, decabromodiphenyl ethane and tetrabromoether are mixed to obtain mixture C, finally, mixture A, mixture B, mixture C and plasticizer are mixed for 12 min-18 min to obtain a powder material; Step 4: Granulation: Granulate the powder material using a granulator to obtain PVC particles; Step 5: Punching: Use laser to punch multiple micro holes on the PVC particles; Step six, soaking: soak the PVC particles in a flame retardant solution. After the soaking is complete, the PVC particles can be taken out to form a flame retardant layer on the PVC particles. Thus, a fire-resistant and flame-retardant PVC material can be obtained.

[0005] As a preferred embodiment of the method for preparing a fire-resistant and flame-retardant PVC material described in the present invention, the raw materials include, by weight: 4-12 parts of polyvinyl chloride, 2-12 parts of calcium stearate, 4-12 parts of acrylate, 4-12 parts of paraffin, 4-12 parts of polypropylene, 1-5 parts of composite stabilizer, 2-4 parts of plasticizer, 2-4 parts of coupling agent, 4-6 parts of antioxidant, 4-8 parts of reinforcing agent, 2-8 parts of preservative, 2-6 parts of decabromodiphenyl ether, 2-6 parts of tetrabromobisphenol A, 2-6 parts of decabromodiphenyl ethane, and 2-6 parts of tetrabromoether.

[0006] As a preferred solution of the method for preparing a fire-resistant and flame-retardant PVC material described in the present invention, the composite stabilizer is a mixture of one or more of calcium stearate, calcium ricinoleate and zinc stearate.

[0007] As a preferred embodiment of the method for preparing a fire-resistant and flame-retardant PVC material according to the present invention, the plasticizer is a mixture of one or more of dibutyl phthalate and dioctyl phthalate.

[0008] As a preferred solution of the method for preparing a fire-resistant and flame-retardant PVC material described in the present invention, the coupling agent is a mixture of one or more of a titanate coupling agent, an aluminate coupling agent, and a borate coupling agent.

[0009] As a preferred embodiment of the method for preparing a fire-resistant and flame-retardant PVC material described in the present invention, the antioxidant is a mixture of one or more of antioxidant 1010, antioxidant DLTP, and antioxidant 164.

[0010] As a preferred solution of the method for preparing a fire-resistant and flame-retardant PVC material described in the present invention, the reinforcing agent is a mixture of one or more of glass fiber, carbon fiber and wollastonite.

[0011] As a preferred embodiment of the method for preparing a fire-resistant and flame-retardant PVC material according to the present invention, the preservative is a mixture of one or more of benzoic acid, glass flakes and potassium sorbate.

[0012] As a preferred embodiment of the method for preparing a fire-resistant flame-retardant PVC material according to the present invention, the preparation process of the flame-retardant solution is as follows: Process 1: heating the polyimide resin, the polyetherketone resin, the phenoxy resin and the flame retardant epoxy resin until the polyimide resin, the polyetherketone resin, the phenoxy resin and the flame retardant epoxy resin become liquid; Process 2: Mixing the curing agent and adhesive; Process 3: The mixtures in process 1 and process 2 are mixed to obtain a flame retardant solution, and the mixture is heated during the mixing to make it liquid.

[0013] As a preferred embodiment of the method for preparing a fire-resistant and flame-retardant PVC material according to the present invention, the mixing time in the second process is 1 min to 5 min, and the mixing time in the third process is 6 min to 12 min.

[0014] Compared with existing technologies: By adding decabromodiphenyl ether, tetrabromobisphenol A, decabromodiphenyl ethane and tetrabromoether to the raw materials, and by forming a flame retardant layer on the inner and outer surfaces of PVC particles, the fire resistance and flame retardancy of PVC materials can be greatly improved, so as to avoid the phenomenon of continuous combustion of PVC materials due to long-term burning to a certain extent, thereby improving safety; in addition, by adding reinforcing agents and preservatives to the raw materials, the tensile strength and anti-corrosion performance of PVC materials can be improved. DETAILED DESCRIPTION

[0015] In order to make the objectives, technical solutions and advantages of the present invention more clear, the embodiments of the present invention will be described in further detail below. Example 1

[0016] The present invention provides a method for preparing a fire-resistant and flame-retardant PVC material, comprising the following specific steps: Step 1, preparation of raw materials: polyvinyl chloride, calcium stearate, acrylate, paraffin, polypropylene, composite stabilizer, plasticizer, coupling agent, antioxidant, enhancer, preservative, decabromodiphenyl ether, tetrabromobisphenol A, decabromodiphenyl ethane, tetrabromoether; The raw materials include, by weight: 4 parts of polyvinyl chloride, 2 parts of calcium stearate, 4 parts of acrylate, 4 parts of paraffin wax, 4 parts of polypropylene, 1 part of composite stabilizer, 2 parts of plasticizer, 2 parts of coupling agent, 4 parts of antioxidant, 4 parts of reinforcing agent, 2 parts of preservative, 2 parts of decabromodiphenyl ether, 2 parts of tetrabromobisphenol A, 2 parts of decabromodiphenyl ethane, and 2 parts of tetrabromoether; The composite stabilizer is a mixture of one or more of calcium stearate, calcium ricinoleate and zinc stearate; the plasticizer is a mixture of one or more of dibutyl phthalate and dioctyl phthalate; the coupling agent is a mixture of one or more of titanate coupling agent, aluminate coupling agent and borate coupling agent; the antioxidant is a mixture of one or more of antioxidant 1010, antioxidant DLTP and antioxidant 164; the reinforcing agent is a mixture of one or more of glass fiber, carbon fiber and wollastonite; the preservative is a mixture of one or more of benzoic acid, glass flakes and potassium sorbate; Step 2, grinding: grinding polyvinyl chloride, calcium stearate, acrylate, paraffin, polypropylene, composite stabilizer, coupling agent, antioxidant, reinforcing agent, preservative, decabromodiphenyl ether, tetrabromobisphenol A, decabromodiphenyl ethane and tetrabromoether to obtain a powdery material; Step 3, mixing: first, polyvinyl chloride, calcium stearate, acrylate, paraffin and polypropylene are mixed for 10 minutes to obtain a mixture A, then, a composite stabilizer, a coupling agent, an antioxidant, a reinforcing agent and a preservative are mixed for 10 minutes to obtain a mixture B, then, decabromodiphenyl ether, tetrabromobisphenol A, decabromodiphenyl ethane and tetrabromoether are mixed to obtain a mixture C, and finally, the mixture A, the mixture B, the mixture C and the plasticizer are mixed for 12 minutes to obtain a powder material; Step 4: Granulation: Granulate the powder material using a granulator to obtain PVC particles; Step 5: Punching: Use laser to punch multiple micro holes on the PVC particles; Step 6, soaking: soaking the PVC particles in a flame retardant solution. After the immersion is complete, the PVC particles can be taken out to form a flame retardant layer on the PVC particles, so that a fire-resistant and flame-retardant PVC material can be obtained; The preparation process of the flame retardant solution is as follows: Process 1: heating the polyimide resin, the polyetherketone resin, the phenoxy resin and the flame retardant epoxy resin until the polyimide resin, the polyetherketone resin, the phenoxy resin and the flame retardant epoxy resin become liquid; Process 2: Mix the curing agent and adhesive for 1 minute; Process 3: The mixtures in process 1 and process 2 are mixed for 6 minutes to obtain a flame retardant solution. During the mixing, the mixture is heated to make it liquid. Example 2

[0017] The present invention provides a method for preparing a fire-resistant and flame-retardant PVC material, comprising the following specific steps: Step 1, preparation of raw materials: polyvinyl chloride, calcium stearate, acrylate, paraffin, polypropylene, composite stabilizer, plasticizer, coupling agent, antioxidant, enhancer, preservative, decabromodiphenyl ether, tetrabromobisphenol A, decabromodiphenyl ethane, tetrabromoether; The raw materials include, by weight: 8 parts of polyvinyl chloride, 7 parts of calcium stearate, 8 parts of acrylate, 8 parts of paraffin, 8 parts of polypropylene, 3 parts of composite stabilizer, 3 parts of plasticizer, 3 parts of coupling agent, 5 parts of antioxidant, 6 parts of reinforcing agent, 5 parts of preservative, 4 parts of decabromodiphenyl ether, 4 parts of tetrabromobisphenol A, 4 parts of decabromodiphenyl ethane, and 4 parts of tetrabromoether; The composite stabilizer is a mixture of one or more of calcium stearate, calcium ricinoleate and zinc stearate; the plasticizer is a mixture of one or more of dibutyl phthalate and dioctyl phthalate; the coupling agent is a mixture of one or more of titanate coupling agent, aluminate coupling agent and borate coupling agent; the antioxidant is a mixture of one or more of antioxidant 1010, antioxidant DLTP and antioxidant 164; the reinforcing agent is a mixture of one or more of glass fiber, carbon fiber and wollastonite; the preservative is a mixture of one or more of benzoic acid, glass flakes and potassium sorbate; Step 2, grinding: grinding polyvinyl chloride, calcium stearate, acrylate, paraffin, polypropylene, composite stabilizer, coupling agent, antioxidant, reinforcing agent, preservative, decabromodiphenyl ether, tetrabromobisphenol A, decabromodiphenyl ethane and tetrabromoether to obtain a powdery material; Step 3, mixing: first, polyvinyl chloride, calcium stearate, acrylate, paraffin and polypropylene are mixed for 13 minutes to obtain a mixture A, then, a composite stabilizer, a coupling agent, an antioxidant, a reinforcing agent and a preservative are mixed for 13 minutes to obtain a mixture B, then, decabromodiphenyl ether, tetrabromobisphenol A, decabromodiphenyl ethane and tetrabromoether are mixed to obtain a mixture C, and finally, the mixture A, the mixture B, the mixture C and the plasticizer are mixed for 14 minutes to obtain a powder material; Step 4: Granulation: Granulate the powder material using a granulator to obtain PVC particles; Step 5: Punching: Use laser to punch multiple micro holes on the PVC particles; Step 6, soaking: soaking the PVC particles in a flame retardant solution. After the immersion is complete, the PVC particles can be taken out to form a flame retardant layer on the PVC particles, so that a fire-resistant and flame-retardant PVC material can be obtained; The preparation process of the flame retardant solution is as follows: Process 1: heating the polyimide resin, the polyetherketone resin, the phenoxy resin and the flame retardant epoxy resin until the polyimide resin, the polyetherketone resin, the phenoxy resin and the flame retardant epoxy resin become liquid; Process 2: Mix the curing agent and adhesive for 3 minutes; Process 3: The mixtures in process 1 and process 2 are mixed for 9 minutes to obtain a flame retardant solution. During the mixing, the mixture is heated to make it liquid. Example 3

[0018] The present invention provides a method for preparing a fire-resistant and flame-retardant PVC material, comprising the following specific steps: Step 1, preparation of raw materials: polyvinyl chloride, calcium stearate, acrylate, paraffin, polypropylene, composite stabilizer, plasticizer, coupling agent, antioxidant, enhancer, preservative, decabromodiphenyl ether, tetrabromobisphenol A, decabromodiphenyl ethane, tetrabromoether; The raw materials include, by weight: 12 parts of polyvinyl chloride, 12 parts of calcium stearate, 12 parts of acrylate, 12 parts of paraffin wax, 12 parts of polypropylene, 5 parts of composite stabilizer, 4 parts of plasticizer, 4 parts of coupling agent, 6 parts of antioxidant, 8 parts of reinforcing agent, 8 parts of preservative, 6 parts of decabromodiphenyl ether, 6 parts of tetrabromobisphenol A, 6 parts of decabromodiphenyl ethane, and 6 parts of tetrabromoether; The composite stabilizer is a mixture of one or more of calcium stearate, calcium ricinoleate and zinc stearate; the plasticizer is a mixture of one or more of dibutyl phthalate and dioctyl phthalate; the coupling agent is a mixture of one or more of titanate coupling agent, aluminate coupling agent and borate coupling agent; the antioxidant is a mixture of one or more of antioxidant 1010, antioxidant DLTP and antioxidant 164; the reinforcing agent is a mixture of one or more of glass fiber, carbon fiber and wollastonite; the preservative is a mixture of one or more of benzoic acid, glass flakes and potassium sorbate; Step 2, grinding: grinding polyvinyl chloride, calcium stearate, acrylate, paraffin, polypropylene, composite stabilizer, coupling agent, antioxidant, reinforcing agent, preservative, decabromodiphenyl ether, tetrabromobisphenol A, decabromodiphenyl ethane and tetrabromoether to obtain a powdery material; Step 3, mixing: first, polyvinyl chloride, calcium stearate, acrylate, paraffin and polypropylene are mixed for 16 minutes to obtain a mixture A, then, a composite stabilizer, a coupling agent, an antioxidant, a reinforcing agent and a preservative are mixed for 16 minutes to obtain a mixture B, then, decabromodiphenyl ether, tetrabromobisphenol A, decabromodiphenyl ethane and tetrabromoether are mixed to obtain a mixture C, and finally, the mixture A, the mixture B, the mixture C and the plasticizer are mixed for 18 minutes to obtain a powder material; Step 4: Granulation: Granulate the powder material using a granulator to obtain PVC particles; Step 5: Punching: Use laser to punch multiple micro holes on the PVC particles; Step 6, soaking: soaking the PVC particles in a flame retardant solution. After the immersion is complete, the PVC particles can be taken out to form a flame retardant layer on the PVC particles, so that a fire-resistant and flame-retardant PVC material can be obtained; The preparation process of the flame retardant solution is as follows: Process 1: heating the polyimide resin, the polyetherketone resin, the phenoxy resin and the flame retardant epoxy resin until the polyimide resin, the polyetherketone resin, the phenoxy resin and the flame retardant epoxy resin become liquid; Process 2: Mix the curing agent and adhesive for 5 minutes; Process 3: The mixtures in process 1 and process 2 are mixed for 12 minutes to obtain a flame retardant solution. During the mixing, the mixture is heated to make it liquid.

[0019] The fire-resistant and flame-retardant PVC materials prepared in the above Examples 1-3 were compared to obtain the following data: Example 1 Example 2 Example 3 Tensile strength 12.65 / MPa 17.32 / MPa 14.01 / MPa Anti-corrosion grade Sa2 Sa2.5 Sa2 Flame retardant grade V-0 V-0 V-0 It can be seen from the above table that the fire-resistant and flame-retardant PVC materials prepared in Examples 1-3 have good performance in tensile strength, anti-corrosion grade and flame retardancy grade. After use, Example 2 has the best effect.

[0020] Although the present invention has been described above with reference to the embodiments, various modifications may be made thereto and parts thereof may be replaced by equivalents without departing from the scope of the present invention. In particular, as long as there is no structural conflict, the various features in the embodiments disclosed in the present invention may be used in combination with each other in any manner, and the fact that these combinations are not exhaustively described in this specification is only for the sake of omitting space and saving resources. Therefore, the present invention is not limited to the specific embodiments disclosed herein, but includes all technical solutions falling within the scope of the claims.

Claims

1. A method for preparing a fire-resistant and flame-retardant PVC material, characterized in that: The specific steps are as follows: Step 1, preparation of raw materials: polyvinyl chloride, calcium stearate, acrylate, paraffin, polypropylene, composite stabilizer, plasticizer, coupling agent, antioxidant, enhancer, preservative, decabromodiphenyl ether, tetrabromobisphenol A, decabromodiphenyl ethane, tetrabromoether; Step 2, grinding: grinding polyvinyl chloride, calcium stearate, acrylate, paraffin, polypropylene, composite stabilizer, coupling agent, antioxidant, reinforcing agent, preservative, decabromodiphenyl ether, tetrabromobisphenol A, decabromodiphenyl ethane and tetrabromoether to obtain a powdery material; Step 3, mixing: first, polyvinyl chloride, calcium stearate, acrylate, paraffin and polypropylene are mixed for 10 min-16 min to obtain mixture A, then, the composite stabilizer, coupling agent, antioxidant, reinforcing agent and preservative are mixed for 10 min-16 min to obtain mixture B, then, decabromodiphenyl ether, tetrabromobisphenol A, decabromodiphenyl ethane and tetrabromoether are mixed to obtain mixture C, finally, mixture A, mixture B, mixture C and plasticizer are mixed for 12 min-18 min to obtain a powder material; Step 4: Granulation: Granulate the powder material using a granulator to obtain PVC particles; Step 5: Punching: Use laser to punch multiple micro holes on the PVC particles; Step six, soaking: soak the PVC particles in a flame retardant solution. After the soaking is complete, the PVC particles can be taken out to form a flame retardant layer on the PVC particles. Thus, a fire-resistant and flame-retardant PVC material can be obtained.

2. The method for preparing a fire-resistant and flame-retardant PVC material according to claim 1, characterized in that: The raw materials include, by weight: 4-12 parts of polyvinyl chloride, 2-12 parts of calcium stearate, 4-12 parts of acrylate, 4-12 parts of paraffin, 4-12 parts of polypropylene, 1-5 parts of composite stabilizer, 2-4 parts of plasticizer, 2-4 parts of coupling agent, 4-6 parts of antioxidant, 4-8 parts of reinforcing agent, 2-8 parts of preservative, 2-6 parts of decabromodiphenyl ether, 2-6 parts of tetrabromobisphenol A, 2-6 parts of decabromodiphenyl ethane, and 2-6 parts of tetrabromoether.

3. The method for preparing a fire-resistant and flame-retardant PVC material according to claim 1, characterized in that: The composite stabilizer is a mixture of one or more of calcium stearate, calcium ricinoleate and zinc stearate.

4. The method for preparing a fire-resistant and flame-retardant PVC material according to claim 1, characterized in that: The plasticizer is a mixture of one or more of dibutyl phthalate and dioctyl phthalate.

5. The method for preparing a fire-resistant and flame-retardant PVC material according to claim 1, characterized in that: The coupling agent is a mixture of one or more of a titanate coupling agent, an aluminate coupling agent and a borate coupling agent.

6. The method for preparing a fire-resistant and flame-retardant PVC material according to claim 1, characterized in that: The antioxidant is one or more of the antioxidant 1010, the antioxidant DLTP, and the antioxidant 164.

7. The method for preparing a fire-resistant and flame-retardant PVC material according to claim 1, characterized in that: The reinforcing agent is a mixture of one or more of glass fiber, carbon fiber and wollastonite.

8. The method for preparing a fire-resistant and flame-retardant PVC material according to claim 1, characterized in that: The preservative is a mixture of one or more of benzoic acid, glass flakes and potassium sorbate.

9. The method for preparing a fire-resistant and flame-retardant PVC material according to claim 1, characterized in that: The preparation process of the flame retardant solution is as follows: Process 1: heating the polyimide resin, the polyetherketone resin, the phenoxy resin and the flame retardant epoxy resin until the polyimide resin, the polyetherketone resin, the phenoxy resin and the flame retardant epoxy resin become liquid; Process 2: Mixing the curing agent and adhesive; Process 3: The mixtures in process 1 and process 2 are mixed to obtain a flame retardant solution, and the mixture is heated during the mixing to make it liquid.

10. The method for preparing a fire-resistant and flame-retardant PVC material according to claim 9, characterized in that: The mixing time in the second process is 1 min to 5 min, and the mixing time in the third process is 6 min to 12 min.