CN112239575A - Sponge rubber and preparation method and application thereof - Google Patents
Sponge rubber and preparation method and application thereof Download PDFInfo
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- CN112239575A CN112239575A CN202011074836.8A CN202011074836A CN112239575A CN 112239575 A CN112239575 A CN 112239575A CN 202011074836 A CN202011074836 A CN 202011074836A CN 112239575 A CN112239575 A CN 112239575A
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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
- C08J9/107—Nitroso compounds
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- A—HUMAN NECESSITIES
- A47—FURNITURE; DOMESTIC ARTICLES OR APPLIANCES; COFFEE MILLS; SPICE MILLS; SUCTION CLEANERS IN GENERAL
- A47C—CHAIRS; SOFAS; BEDS
- A47C27/00—Spring, stuffed or fluid mattresses or cushions specially adapted for chairs, beds or sofas
- A47C27/14—Spring, stuffed or fluid mattresses or cushions specially adapted for chairs, beds or sofas with foamed material inlays
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- C—CHEMISTRY; METALLURGY
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- C08J11/04—Recovery or working-up of waste materials of polymers
- C08J11/10—Recovery or working-up of waste materials of polymers by chemically breaking down the molecular chains of polymers or breaking of crosslinks, e.g. devulcanisation
- C08J11/16—Recovery or working-up of waste materials of polymers by chemically breaking down the molecular chains of polymers or breaking of crosslinks, e.g. devulcanisation by treatment with inorganic material
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- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
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- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
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- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/0061—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof characterized by the use of several polymeric components
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- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/0095—Mixtures of at least two compounding ingredients belonging to different one-dot groups
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- 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
- C08J9/104—Hydrazines; Hydrazides; Semicarbazides; Semicarbazones; Hydrazones; Derivatives thereof
- C08J9/105—Hydrazines; Hydrazides; Semicarbazides; Semicarbazones; Hydrazones; Derivatives thereof containing sulfur
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- C08J2309/00—Characterised by the use of homopolymers or copolymers of conjugated diene hydrocarbons
- C08J2309/06—Copolymers with styrene
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- C08J2383/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
- C08J2383/04—Polysiloxanes
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- C08J2423/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2423/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2423/04—Homopolymers or copolymers of ethene
- C08J2423/08—Copolymers of ethene
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- C08J2471/00—Characterised by the use of polyethers obtained by reactions forming an ether link in the main chain; Derivatives of such polymers
- C08J2471/02—Polyalkylene oxides
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- 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
- C08J2483/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
- C08J2483/04—Polysiloxanes
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/62—Plastics recycling; Rubber recycling
Abstract
The application relates to the field of sponge rubber, and particularly discloses sponge rubber and a preparation method and application thereof. A sponge rubber is prepared from the following raw materials: styrene butadiene rubber, carbon black, clay, EVA recycled powder, a plasticizer, a foaming agent, a crosslinking agent and an auxiliary agent, wherein the mesh number of the EVA recycled powder is more than 60 meshes; the preparation method comprises the following steps: and (3) performing primary refining, A refining, B refining and foaming in sequence to obtain the sponge rubber. The sponge rubber of this application can be used to make sponge mattress. The sponge rubber has the advantages of low shrinkage, excellent mechanical property and good hand feeling.
Description
Technical Field
The application relates to the field of sponge rubber, in particular to sponge rubber and a preparation method and application thereof.
Background
The sponge rubber is a porous structural material with pores distributed throughout the material. It has low density, excellent elasticity and flexibility, high damping, sound isolating and heat insulating performance. The products are various in types and shapes, and are widely applied to sealing, shock absorption, clothes, shoemaking, household appliances, printing and dyeing, home decoration and other aspects, and in the aspect of home decoration, the sponge rubber is commonly used as a sponge mattress.
At present, natural rubber, styrene butadiene rubber or butadiene rubber is usually selected as the sponge rubber, and the styrene butadiene rubber is low in cost and good in forming effect, so that the sponge rubber is widely applied.
However, the shrinkage rate of the existing sponge rubber is high, namely, after the formed sponge rubber is placed for 20 days, the shrinkage rate exceeds 4.2%, and the quality of the mattress made of the sponge rubber is poor.
Disclosure of Invention
In order to obtain the sponge rubber with low shrinkage rate, the application provides the sponge rubber and a preparation method and application thereof.
In a first aspect, the present application provides a sponge rubber, which adopts the following technical scheme:
the sponge rubber is prepared from the following raw materials in parts by weight:
100 parts of styrene butadiene rubber;
20-40 parts of carbon black;
20-40 parts of clay;
10-20 parts of EVA (ethylene-vinyl acetate) regenerated powder;
20-40 parts of a plasticizer;
12-16 parts of a foaming agent;
3-5 parts of a crosslinking agent;
7-11 parts of an auxiliary agent;
the mesh number of the EVA regeneration powder is more than 60 meshes.
By adopting the technical scheme, when the sponge rubber is prepared, the styrene butadiene rubber has the advantages of good processability, low contractibility and the like, and the clay and the carbon black are cooperated, so that the strength of the sponge rubber can be enhanced, and the sponge rubber has better mechanical properties. The plasticizer can improve the plasticity of the sponge rubber and improve the strength of the sponge rubber. The addition of the EVA regeneration powder can be cooperated with carbon black and the like to increase the strength of the sponge rubber and reduce the addition of the carbon black. In addition, the EVA regenerated powder can effectively reduce the shrinkage rate of the sponge rubber. The mesh number of the EVA recycled powder is more than 60 meshes, and if the mesh number of the EVA recycled powder is less than 60 meshes, the particle size of the EVA recycled powder is too large, the EVA recycled powder cannot be uniformly mixed after the styrene butadiene rubber is added, and the mechanical property of the sponge rubber is reduced due to the fact that the EVA recycled powder cannot be uniformly mixed. In addition, owing to adopt EVA regeneration powder, can reduce the waste of abandonment EVA, improve EVA's rate of recovery, comparatively green. The addition of the cross-linking agent can form chemical bonds among molecules in the raw materials, and effectively improve the strength and elasticity of the rubber. The foaming agent can make the sponge rubber pore-forming. The auxiliary agent can be improved by adding corresponding auxiliary agent according to the required performance. The sponge rubber prepared from the raw materials has low shrinkage rate, and the shrinkage rate is less than 3.6% in 20 days.
Preferably, the plasticizer is naphthenic oil or aromatic oil.
By adopting the technical scheme, when the naphthenic oil or the aromatic oil is used as the plasticizer, the naphthenic oil or the aromatic oil is easy to disperse in the sponge rubber, and besides, the naphthenic oil and the aromatic oil have good plasticizing effect, and besides, the naphthenic oil and the aromatic oil can be well mixed with the EVA reclaimed powder.
Preferably, the blowing agent is blowing agent H.
By adopting the technical scheme, the foaming agent H can have a good foaming effect and can be well mixed in the sponge rubber.
Preferably, the crosslinking agent is dicumyl peroxide.
By adopting the technical scheme, the dicumyl peroxide is used as the cross-linking agent, and has a better cross-linking effect.
Preferably, the auxiliary agent is an anti-aging agent and an active agent, wherein the anti-aging agent is 4-6 parts by weight, and the active agent is 3-5 parts by weight.
By adopting the technical scheme, after the sponge rubber is made into a product, the service life is expected to be longer, the replacement frequency is reduced, and at the moment, the anti-aging agent can be added to prolong the service life of the sponge rubber product. And the addition of the activating agent can reduce the time required by vulcanization during the molding of the sponge rubber, reduce the vulcanization time and increase the preparation efficiency.
Preferably, the antioxidant is p-phenylenediamine.
By adopting the technical scheme, the p-phenylenediamine can be used as an anti-aging agent and can be well mixed with the styrene butadiene rubber and the EVA regeneration powder.
Preferably, the active agent is one or a mixture of zinc oxide and stearic acid.
By adopting the technical scheme, the zinc oxide and the stearic acid are uniformly mixed in the sponge rubber, so that the vulcanization speed of the sponge rubber can be increased, and the production efficiency is improved.
Preferably, the rubber also comprises 5-10 parts of regenerated silicon rubber, which is prepared by the following method:
the method comprises the following steps: crushing the recovered silicon rubber, soaking the crushed silicon rubber in a sodium hydroxide aqueous solution, performing ultrasonic treatment, and drying to obtain pretreated recovered silicon rubber;
step two: adding polyoxypropylene glycol into the pretreated recycled silicone rubber obtained in the step one, wherein the weight ratio of the polyoxypropylene glycol to the silicone rubber is 1: (0.2-0.5), stirring uniformly, heating to 50-60 ℃ to obtain a mixture, adding hexamethylenetetramine into the mixture while the mixture is hot, and stirring, wherein the weight ratio of the hexamethylenetetramine to the hexamethylenetetramine is 1: (0.02-0.08), and cooling to room temperature to obtain the regenerated silicone rubber.
By adopting the technical scheme, after the recovered silicone rubber is treated, the recovered silicone rubber is placed in an alkaline solution for ultrasonic treatment, so that chemical bonds between the silicone rubber and part of additives in the silicone rubber can be effectively broken, in addition, due to the alkaline solution, the chemical bonds are more easily broken during ultrasonic treatment, more linear oligomeric dimethyl siloxane is obtained, then polyoxypropylene glycol is added into the obtained pretreated recovered silicone rubber, and the silicone rubber and the polyoxypropylene glycol are uniformly mixed under the condition of temperature rise to obtain a mixture. And adding hexamethylenetetramine to wrap the surface of the mixture and obtain the regenerated silicon rubber. The obtained regenerated silicon rubber is easy to disperse in the sponge rubber, and in the modification process, the viscosity of the regenerated silicon rubber is reduced, and the influence on the mechanical property of the sponge rubber is reduced. In addition, the surface of the regenerated silicon rubber is provided with two chemical coating layers, when the sponge rubber is prepared, the first chemical coating layer of the hexamethylenetetramine is uniformly dispersed in the styrene butadiene rubber, and then the second chemical coating layer of the polypropylene oxide glycol is released in the heating process, so that the sponge rubber has a good foaming effect in the foaming process, the foaming is more dense, and in addition, the obtained sponge rubber has good resilience and low shrinkage. In addition, the regenerated silicon rubber can be used as a filler to improve the mechanical property of the sponge rubber.
Preferably, the regenerated silicone rubber is prepared by the following method:
the method comprises the following steps: crushing the recovered silicon rubber, soaking the crushed silicon rubber in a 3-5% sodium hydroxide aqueous solution, performing ultrasonic treatment for 10-20min, and drying to obtain pretreated recovered silicon rubber;
step two: adding polyoxypropylene glycol into the pretreated recycled silicone rubber obtained in the step one, wherein the weight ratio of the polyoxypropylene glycol to the silicone rubber is 1: (0.2-0.5), uniformly stirring, heating to 50-60 ℃, stirring while heating at the heating rate of 0.5-1.5 ℃/min to obtain a mixture, adding hexamethylenetetramine into the mixture while the mixture is hot, stirring for 10-20min, wherein the weight ratio of the hexamethylenetetramine to the hexamethylenetetramine is 1: (0.02-0.08), and cooling to room temperature to obtain the regenerated silicone rubber.
By adopting the technical scheme, the regenerated silicone rubber prepared by the method has better dispersibility, and the shrinkage rate of the sponge rubber can be reduced while the mechanical property of the sponge rubber is improved.
Further, the weight ratio of the EVA regeneration powder to the regenerated silicone rubber is 5: 1.
By adopting the technical scheme, when the weight ratio of the EVA recycled powder to the recycled silicon rubber is 5:1, the prepared sponge rubber has better mechanical property and low shrinkage rate.
Further, the sponge rubber is prepared from the following raw materials in parts by weight:
100 parts of styrene butadiene rubber;
30 parts of carbon black;
30 parts of clay;
10-20 parts of EVA (ethylene-vinyl acetate) regenerated powder;
30 parts of naphthenic oil;
14 parts of a foaming agent H;
4 parts of dicumyl peroxide;
5 parts of p-phenylenediamine;
4 parts of stearic acid;
3 parts of regenerated silicone rubber.
By adopting the technical scheme, when the sponge rubber is prepared according to the proportion, the prepared sponge rubber has better mechanical property and low shrinkage rate.
In a second aspect, the present application provides a preparation method of a sponge rubber, which adopts the following technical scheme:
a preparation method of sponge rubber comprises the following steps:
the method comprises the following steps: performing masterbatch, namely uniformly mixing styrene butadiene rubber, carbon black, clay, EVA (ethylene-vinyl acetate copolymer) regenerated powder and 10-30% of total plasticizer, and mixing to obtain masterbatch;
step two: mixing A, adding the rest plasticizer and auxiliary agent into the master batch obtained in the step one, and mixing to obtain rubber A;
step three: b, mixing, namely adding a foaming agent and a cross-linking agent into the rubber compound A obtained in the step two, and mixing to obtain sponge rubber;
step four: foaming, namely vulcanizing the sponge rubber obtained in the step three, and forming to obtain the sponge rubber.
By adopting the technical scheme, in the process of preparing the sponge rubber, the master batch is firstly carried out, the styrene-butadiene rubber, the plasticizer, the carbon black, the EVA recycled powder and other substances which are not easy to disperse are mixed, then the auxiliary agent and the rest plasticizer are added, the other substances except the foaming agent and the cross-linking agent are completely mixed together to form the rubber A, then the foaming agent and the cross-linking agent are added into the rubber A, the rubber A is mixed to form the sponge rubber, and the sponge rubber can be stored and vulcanized when the sponge rubber is required to be formed. The method is simple and can uniformly mix all the substances in a short time.
Preferably, the step one is specifically: styrene butadiene rubber, carbon black, clay, EVA recycled powder and 10-30% of total plasticizer are uniformly mixed and mixed, the mixing temperature is 135-150 ℃, and the mixing time is 270-400s, so as to prepare the master batch.
By adopting the technical scheme, in the step one, the mixing temperature is 135-150 ℃, the mixing time is 270-400s, and the raw materials can be pre-mixed, so that substances which are easy to mix and difficult to mix are uniformly mixed at a slightly higher temperature.
Preferably, the second step is specifically: and (3) adding the rest plasticizer and auxiliary agent into the master batch obtained in the step one, and mixing at the mixing temperature of 115-125 ℃ for 7-10min to obtain the rubber A.
By adopting the technical scheme, in the step two, the residual plasticizer and the auxiliary agent are added into the pre-mixed raw materials, and the mixture is mixed at a lower mixing temperature relative to the mixing temperature in the step one, so that uniform rubber A is obtained.
Preferably, the third step is specifically: and (3) adding a foaming agent and a cross-linking agent into the rubber compound A obtained in the step two, and mixing at the temperature of 95-105 ℃ for 6-10min to obtain the sponge rubber.
By adopting the technical scheme, in the third step, the foaming agent and the cross-linking agent are added into the pre-mixed raw materials for mixing, and the mixing temperature is lower than that in the second step, so that the uniform sponge rubber is obtained.
Preferably, the step four specifically comprises: and (3) carrying out first-stage vulcanization on the sponge rubber prepared in the third step, wherein the vulcanization temperature is 130-.
By adopting the technical scheme, in the fourth step, two-stage vulcanization is adopted, the vulcanization temperature of the first stage is lower than that of the second stage, and the first stage vulcanization is used for carrying out micro-foaming. The sponge rubber is pre-shaped, then the second-stage vulcanization is carried out, and the foaming is carried out, so that the rubber obtained after vulcanization is better in forming.
Preferably, the sponge rubber is prepared by the following method:
the method comprises the following steps: and (2) performing masterbatch, namely uniformly mixing styrene butadiene rubber, carbon black, clay, EVA (ethylene-vinyl acetate) regenerated powder and 10-30% of total plasticizer, and mixing at the mixing temperature of 140 ℃ for 360 seconds to obtain the masterbatch.
Step two: and A, mixing, namely adding the rest plasticizer and auxiliary agent into the master batch obtained in the step one, and mixing at the mixing temperature of 120 ℃ for 8min to obtain the rubber A.
Step three: and B, mixing, namely adding a foaming agent and a cross-linking agent into the rubber compound A obtained in the step two, and mixing at the mixing temperature of 100 ℃ for 8min to obtain the sponge rubber.
Step four: and (3) foaming, namely performing first-stage vulcanization on the sponge rubber prepared in the step three at the vulcanization temperature of 135 ℃ for 28min, and then performing second-stage vulcanization at the vulcanization temperature of 165 ℃ for 26 min.
By adopting the technical scheme, when the sponge rubber is prepared by adopting the steps and the conditions, the sponge rubber has better mechanical property and lower shrinkage rate.
Preferably, the first step is specifically: styrene butadiene rubber, carbon black, clay, EVA recycled powder, recycled silicon rubber and 10-30% of total plasticizer are uniformly mixed and mixed, the mixing temperature is 135-150 ℃, and the mixing time is 270-400s, so as to prepare the master batch.
By adopting the technical scheme, when the regenerated silicon rubber needs to be added, the master batch prepared by adopting the steps and the conditions is more uniform.
Preferably, the sponge rubber is prepared by the following method:
the method comprises the following steps: and (2) performing master batch, namely uniformly mixing styrene butadiene rubber, carbon black, clay, EVA (ethylene vinyl acetate) regenerated powder, regenerated silicon rubber and 10-30% of total plasticizer, and mixing at 145 ℃ for 380 seconds to obtain the master batch.
Step two: and A, mixing, namely adding the rest plasticizer and auxiliary agent into the master batch obtained in the step one, and mixing at the mixing temperature of 120 ℃ for 8min to obtain the rubber A.
Step three: and B, mixing, namely adding a foaming agent and a cross-linking agent into the rubber compound A obtained in the step two, and mixing at the mixing temperature of 100 ℃ for 8min to obtain the sponge rubber.
Step four: and (3) foaming, namely performing first-stage vulcanization on the sponge rubber prepared in the step three at the vulcanization temperature of 135 ℃ for 28min, and then performing second-stage vulcanization at the vulcanization temperature of 165 ℃ for 26 min.
By adopting the technical scheme, when the regenerated silicon rubber needs to be added, the sponge rubber is prepared by adopting the steps and the conditions, and has better mechanical property and lower shrinkage rate.
In a third aspect, the application provides a sponge mattress, which adopts the following technical scheme:
a sponge mattress is cut from the sponge rubber.
By adopting the technical scheme, when the sponge mattress is prepared, the obtained sponge rubber is directly cut into corresponding sizes, and the sponge mattress can be obtained. If the size is just the required size, the sponge rubber is directly used as the sponge mattress without cutting. And the obtained sponge mattress has smaller shrinkage rate.
Preferably, the sponge mattress is prepared by the following method:
and cutting the sponge rubber, and then wrapping and sewing the fabric on the surface of the cut sponge rubber to obtain the sponge mattress with the required size.
Through adopting above-mentioned technical scheme, when preparing the sponge mattress, can have the cloth with the sponge mattress parcel of suitable size, obtain the sponge mattress.
In summary, the present application has the following beneficial effects:
1. as the styrene butadiene rubber, the carbon black, the EVA regeneration powder, the plasticizer, the auxiliary agent, the foaming agent and the cross-linking agent are adopted, and the EVA regeneration powder is added, the obtained sponge rubber has better mechanical property, the using amount of the carbon black is reduced, and the shrinkage rate of the sponge rubber is effectively reduced.
2. The regenerated silicone rubber is preferably added, and the surface of the regenerated silicone rubber is coated with two chemical coating layers, so that the regenerated silicone rubber is easily dispersed in the sponge rubber, and the prepared sponge rubber has good resilience and low contractility.
3. According to the method, the sponge rubber is obtained by sequentially carrying out primary smelting, A smelting, B smelting and foaming, and the preparation process is simple.
4. The sponge mattress has better shrinkage rate and better mechanical property.
Detailed Description
The present application will be described in further detail with reference to examples.
In the following preparation examples and examples, each raw material was commercially available, and some raw materials were as shown in table 1.
Obtaining EVA regeneration powder: the waste materials generated in the preparation of EVA shoe soles are collected from shoe factories and smashed, so that the mesh number is larger than 60 meshes, and can be between 60 and 300 meshes.
Table 1: partial raw material source table
Preparation example
Preparation example 1
The regenerated silicon rubber is prepared by the following steps:
the method comprises the following steps: crushing 10kg of recycled silicon rubber, soaking the crushed recycled silicon rubber with the mesh number of 1000 meshes in a 3% sodium hydroxide aqueous solution, performing ultrasonic treatment for 20min, and drying to obtain pretreated recycled silicon rubber;
step two: adding polyoxypropylene glycol into the pretreated recycled silicone rubber obtained in the step one, wherein the weight ratio of the polyoxypropylene glycol to the silicone rubber is 1: 0.5, uniformly stirring, heating to 60 ℃, stirring while heating, wherein the heating rate is 0.5 ℃/min to obtain a mixture, adding hexamethylenetetramine into the mixture while the mixture is hot, stirring for 20min, and the weight ratio of the hexamethylenetetramine to the hexamethylenetetramine is 1: 0.02, cooling to room temperature to obtain the regenerated silicon rubber.
Preparation example 2
The regenerated silicon rubber is prepared by the following steps:
the method comprises the following steps: crushing 10kg of recycled silicon rubber, wherein the mesh number of the crushed recycled silicon rubber is 600 meshes, soaking the crushed recycled silicon rubber in a 5% sodium hydroxide aqueous solution, performing ultrasonic treatment for 10min, and drying to obtain pretreated recycled silicon rubber;
step two: adding polyoxypropylene glycol into the pretreated recycled silicone rubber obtained in the step one, wherein the weight ratio of the polyoxypropylene glycol to the silicone rubber is 1: 0.2, uniformly stirring, heating to 500 ℃, stirring while heating, wherein the heating rate is 1.5 ℃/min to obtain a mixture, adding hexamethylenetetramine into the mixture while the mixture is hot, stirring for 10min, and the weight ratio of the hexamethylenetetramine to the hexamethylenetetramine is 1: and 0.08, cooling to room temperature to obtain the regenerated silicon rubber.
Preparation example 3
The regenerated silicon rubber is prepared by the following steps:
the method comprises the following steps: crushing 10kg of recycled silicon rubber, soaking the crushed recycled silicon rubber with the mesh number of 800 meshes in a 4% sodium hydroxide aqueous solution, performing ultrasonic treatment for 15min, and drying to obtain pretreated recycled silicon rubber;
step two: adding polyoxypropylene glycol into the pretreated recycled silicone rubber obtained in the step one, wherein the weight ratio of the polyoxypropylene glycol to the silicone rubber is 1: 0.4, uniformly stirring, heating to 55 ℃, stirring while heating, wherein the heating rate is 1.0 ℃/min to obtain a mixture, adding hexamethylenetetramine into the mixture while the mixture is hot, stirring for 15min, and the weight ratio of the hexamethylenetetramine to the hexamethylenetetramine is 1: 0.05, and cooling to room temperature to obtain the regenerated silicon rubber.
Examples
Example 1
A sponge rubber is prepared by the following steps:
the method comprises the following steps: and (3) performing master batch, namely uniformly mixing styrene butadiene rubber, carbon black, clay, EVA recycled powder and 10-30% of total plasticizer in weight shown in the table 2, and mixing at the mixing temperature of 140 ℃ for 360 seconds to obtain the master batch.
Step two: and A, mixing, namely adding the rest plasticizer, the antioxidant and the activator with the weight shown in the table 2 into the master batch obtained in the step one, and mixing at the mixing temperature of 120 ℃ for 8min to obtain the rubber A.
Step three: and B, mixing, namely adding the foaming agent and the cross-linking agent with the weight shown in the table 2 into the rubber compound A obtained in the step two, and mixing at the mixing temperature of 100 ℃ for 8min to obtain the sponge rubber.
Step four: and (3) foaming, namely performing first-stage vulcanization on the sponge rubber prepared in the step three at the vulcanization temperature of 135 ℃ for 28min, and then performing second-stage vulcanization at the vulcanization temperature of 165 ℃ for 26 min.
Wherein, the plasticizer is naphthenic oil; the anti-aging agent is selected from p-phenylenediamine; the activating agent is zinc oxide; the foaming agent is selected from foaming agent H; the cross-linking agent is dicumyl peroxide.
Examples 2 to 3
A sponge rubber was obtained as shown in Table 2, which was different from example 1 in the weight of each raw material.
Example 4
The sponge rubber is different from the sponge rubber in example 1 in that the weight of each raw material is shown in Table 2, the plasticizer is aromatic oil, the crosslinking agent is tetramethyl thiuram disulfide, and the foaming agent is OBSH.
Example 5
A sponge rubber, which is different from the sponge rubber in example 4 in that the first step is specifically as follows: styrene butadiene rubber, carbon black, clay, EVA recycled powder and recycled silicone rubber which are shown in the weight table 2 are evenly mixed with 20 percent of total plasticizer and are mixed for 380s at the mixing temperature of 145 ℃ to prepare the master batch.
Examples 6 to 10
The sponge rubber is different from the sponge rubber in example 3 in that the weight of each raw material is shown in Table 2, and the first step is as follows: styrene butadiene rubber, carbon black, clay, EVA recycled powder and recycled silicone rubber which are shown in the weight table 2 are evenly mixed with 20 percent of total plasticizer and are mixed for 380s at the mixing temperature of 145 ℃ to prepare the master batch.
Example 11
A sponge rubber, which is different from the sponge rubber in the embodiment 10, in the step one, the plasticizer is added to be 10 percent of the total plasticizer, the mixing temperature is 135 ℃, and the mixing time is 400 s; in the second step, the mixing temperature is 125 ℃, and the mixing time is 7 min; in the third step, the mixing temperature is 105 ℃, the mixing time is 10min, in the fourth step, the vulcanization temperature of the first stage vulcanization is 130 ℃, the vulcanization time is 30min, the vulcanization temperature of the second stage vulcanization is 170 ℃, and the vulcanization time is 24 min.
Example 12
A sponge rubber, which is different from the sponge rubber in the embodiment 10 in that in the step one, the plasticizer is added to be 30 percent of the total plasticizer, the mixing temperature is 150 ℃, and the mixing time is 270 s; in the second step, the mixing temperature is 115 ℃ and the mixing time is 10 min; in the third step, the mixing temperature is 95 ℃, and the mixing time is 10 min; in the fourth step, the vulcanization temperature of the first stage vulcanization is 140 ℃, the vulcanization time is 26min, the vulcanization temperature of the second stage vulcanization is 160 ℃, and the vulcanization time is 28 min.
Comparative example
Comparative example 1
A sponge rubber, which differs from example 3 in that no EVA recycled powder is added.
Comparative example 2
A sponge rubber was distinguished from comparative example 1 in that the weight of the plasticizer was 75 kg.
Comparative examples 3 to 4
A sponge rubber was obtained as shown in Table 2, which was different from example 3 in the weight of each raw material.
Comparative example 5
A sponge rubber was distinguished from example 10 in that no EVA recycled powder was added.
Table 2: raw material proportioning meter
Application example 1
A sponge mattress is cut from the sponge rubber obtained in example 3 to form a sponge mattress with a thickness of 3-10cm, in this example 5 cm.
Application example 2
A sponge mattress is different from the application example 1 in that a layer of cloth is sewn on the surface of cut sponge rubber, and the sponge mattress is formed by wrapping the cloth on the surface of the sponge rubber.
Performance test
1. Shrinkage test, the sponge rubbers prepared in examples 1 to 12 and comparative examples 1 to 5 were placed under natural conditions, and the volume of the sponge rubbers was measured after 1, 3, 5, 7, 10, 15, and 20 days, respectively, to calculate the shrinkage, and the test results are shown in table 3.
2. And (3) hand feeling test, namely touching the surface of the sponge rubber in a hand touch mode to measure the roughness, wherein the test results are shown in table 4.
3. Tensile strength test the tensile strength test was carried out on the sponge rubbers obtained in examples 1 to 12 and comparative examples 1 to 5 according to the method described in GB/T528-2009 test Standard, and the test results are shown in Table 4.
4. Elongation, the sponge rubbers obtained in examples 1 to 12 and comparative examples 1 to 5 were subjected to elongation test according to the method described in GB/T528-2009 test Standard, and the test results are shown in Table 4.
Table 3: shrinkage test data
Table 4: tensile strength, hand feel and elongation test data
| Tensile Strength (kg/cm)2) | Hand feeling | Elongation (%) | |
| Example 1 | 5.2 | Fine and smooth hand feeling | 202 |
| Example 2 | 5.1 | Fine and smooth hand feeling | 201 |
| Example 3 | 5.2 | Fine and smooth hand feeling | 202 |
| Example 4 | 5.1 | Fine and smooth hand feeling | 200 |
| Example 5 | 5.2 | Fine and smooth hand feeling | 203 |
| Example 6 | 5.2 | Fine and smooth hand feeling | 202 |
| Example 7 | 5.2 | Fine and smooth hand feeling | 203 |
| Example 8 | 5.2 | Fine and smooth hand feeling | 204 |
| Example 9 | 5.2 | Fine and smooth hand feeling | 204 |
| Example 10 | 5.3 | Fine and smooth hand feeling | 205 |
| Example 11 | 5.3 | Fine and smooth hand feeling | 204 |
| Example 12 | 5.2 | Fine and smooth hand feeling | 204 |
| Comparative example 1 | 4.9 | Fine and smooth hand feeling | 195 |
| Comparative example 2 | 4.7 | Fine and smooth hand feeling | 192 |
| Comparative example 3 | 4.3 | Rough hand feeling | 182 |
| Comparative example 4 | 5.0 | Fine and smooth hand feeling | 196 |
| Comparative example 5 | 5.0 | Fine and smooth hand feeling | 197 |
In addition to the fact that the sponge rubber obtained by adding the regenerated EVA powder has a good shrinkage property when the sponge rubber is prepared, as can be seen by combining examples 1 to 4 and comparative example 1 with table 3, the mechanical properties of the sponge rubber can be made good by combining table 4 with the addition of the regenerated EVA powder.
By combining examples 1-4 and comparative example 2 and tables 3-4, it can be seen that the addition of plasticizer can be greatly reduced when preparing the sponge rubber after adding the regenerated EVA powder, and the obtained sponge rubber has good mechanical properties.
When the EVA recycled powder is excessively added, the foaming effect of the resulting sponge rubber is poor and the hand feeling is poor, as can be seen by combining example 3 and comparative examples 3 to 4 with tables 3 to 4. When the amount of the EVA recycled powder is too small, the shrinkage rate of the prepared sponge rubber is larger.
It can be seen from the combination of examples 4 to 10 and comparative example 5 and tables 3 to 4 that when only the reclaimed silicone rubber was added and no EVA reclaimed powder was added, the shrinkage of the resulting sponge rubber was slightly reduced, but not much.
It can be seen from the combination of examples 1 to 12 and tables 3 to 4 that the shrinkage of each example after 20 days of molding is less than 4.0%, and even 3.5%, and the shrinkage after 1 day of molding is less than 2.3%, which indicates that the shrinkage is small and the increase of the shrinkage is small during the molding to be stable. Indicating that the sponge rubber described in this application has a lower shrinkage. Further, examples 1 to 4 and examples 5 to 12 show that when the regenerated silicone rubber is added, sponge rubber having better properties can be obtained.
As shown in the comparison of examples 3-6, when the plasticizer is naphthenic oil, the activator is zinc oxide, the foaming agent is foaming agent H, and the crosslinking agent is dicumyl peroxide, the obtained sponge rubber has better performances.
Examples 6, 7 and 10 show that the properties of the sponge rubber obtained when the reclaimed silicone rubber obtained in preparation example 3 was used were better. Compared with examples 8-10, when the weight ratio of the EVA recycled powder to the recycled silicone rubber is 5:1, the prepared sponge rubber has better performances. Examples 10-12 have lower shrinkage and better performance than the sponge rubber prepared using the parameters of example 10. Compared with examples 5-10, the sponge rubber prepared in examples 1-4 has lower shrinkage and better mechanical properties after the addition of the regenerated silicone rubber.
The present embodiment is only for explaining the present application, and it is not limited to the present application, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present application.
Claims (10)
1. The sponge rubber is characterized by being prepared from the following raw materials in parts by weight:
100 parts of styrene butadiene rubber;
20-40 parts of carbon black;
20-40 parts of clay;
10-20 parts of EVA (ethylene-vinyl acetate) regenerated powder;
20-40 parts of a plasticizer;
12-16 parts of a foaming agent;
3-5 parts of a crosslinking agent;
7-11 parts of an auxiliary agent;
the mesh number of the EVA regeneration powder is more than 60 meshes.
2. The sponge rubber according to claim 1, wherein: the plasticizer is naphthenic oil or aromatic oil.
3. The sponge rubber according to claim 1, wherein: the foaming agent is a foaming agent H.
4. The sponge rubber according to claim 1, wherein: the cross-linking agent is dicumyl peroxide.
5. The sponge rubber according to claim 1, wherein: the auxiliary agent comprises 4-6 parts of anti-aging agent and 3-5 parts of active agent.
6. The sponge rubber according to any one of claims 1 to 5, wherein: the rubber material also comprises 5-10 parts of regenerated silicon rubber, which is prepared by the following method:
the method comprises the following steps: crushing the recovered silicon rubber, soaking the crushed silicon rubber in a sodium hydroxide aqueous solution, performing ultrasonic treatment, and drying to obtain pretreated recovered silicon rubber;
step two: adding polyoxypropylene glycol into the pretreated recycled silicone rubber obtained in the step one, wherein the weight ratio of the polyoxypropylene glycol to the silicone rubber is 1: (0.2-0.5), stirring uniformly, heating to 50-60 ℃ to obtain a mixture, adding hexamethylenetetramine into the mixture while the mixture is hot, and stirring, wherein the weight ratio of the hexamethylenetetramine to the hexamethylenetetramine is 1: (0.02-0.08), and cooling to room temperature to obtain the regenerated silicone rubber.
7. The preparation method of the sponge rubber is characterized by comprising the following steps:
the method comprises the following steps: performing masterbatch, namely uniformly mixing styrene butadiene rubber, carbon black, clay, EVA (ethylene-vinyl acetate copolymer) regenerated powder and 10-30% of total plasticizer, and mixing to obtain masterbatch;
step two: mixing A, adding the rest plasticizer and auxiliary agent into the master batch obtained in the step one, and mixing to obtain rubber A;
step three: b, mixing, namely adding a foaming agent and a cross-linking agent into the rubber compound A obtained in the step two, and mixing to obtain sponge rubber;
step four: foaming, namely vulcanizing the sponge rubber obtained in the step three, and forming to obtain the sponge rubber.
8. The sponge rubber according to claim 7, wherein: the fourth step is specifically as follows: and (3) carrying out first-stage vulcanization on the sponge rubber prepared in the third step, wherein the vulcanization temperature is 130-.
9. A sponge rubber according to claim 7 or 8, wherein: the first step is as follows: styrene butadiene rubber, carbon black, clay, EVA recycled powder, recycled silicon rubber and 10-30% of total plasticizer are uniformly mixed and mixed, the mixing temperature is 135-150 ℃, and the mixing time is 270-400s, so as to prepare the master batch.
10. A sponge mattress is characterized in that the sponge mattress is made of the sponge rubber through cutting.
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