CN112521658A - Pasty organic peroxide crosslinking agent and compounding process thereof - Google Patents

Pasty organic peroxide crosslinking agent and compounding process thereof Download PDF

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Publication number
CN112521658A
CN112521658A CN202011425730.8A CN202011425730A CN112521658A CN 112521658 A CN112521658 A CN 112521658A CN 202011425730 A CN202011425730 A CN 202011425730A CN 112521658 A CN112521658 A CN 112521658A
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water
dibenzoyl peroxide
crosslinking agent
desensitizer
weight
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Inventor
王文博
李庆朝
杜孟成
马德龙
李剑波
黄存影
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Shandong Yanggu Huatai Chemical Co Ltd
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Shandong Yanggu Huatai Chemical Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00Use of organic ingredients
    • C08K5/04Oxygen-containing compounds
    • C08K5/14Peroxides
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/24Acids; Salts thereof
    • C08K3/26Carbonates; Bicarbonates
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/34Silicon-containing compounds
    • C08K3/346Clay
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/34Silicon-containing compounds
    • C08K3/36Silica
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00Use of organic ingredients
    • C08K5/04Oxygen-containing compounds
    • C08K5/10Esters; Ether-esters
    • C08K5/11Esters; Ether-esters of acyclic polycarboxylic acids
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L23/00Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
    • C08L23/02Compositions 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
    • C08L23/16Elastomeric ethene-propene or ethene-propene-diene copolymers, e.g. EPR and EPDM rubbers
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L23/00Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
    • C08L23/02Compositions 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
    • C08L23/18Homopolymers or copolymers of hydrocarbons having four or more carbon atoms
    • C08L23/20Homopolymers or copolymers of hydrocarbons having four or more carbon atoms having four to nine carbon atoms
    • C08L23/22Copolymers of isobutene; Butyl rubber ; Homo- or copolymers of other iso-olefins
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L83/00Compositions 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; Compositions of derivatives of such polymers
    • C08L83/04Polysiloxanes
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/24Acids; Salts thereof
    • C08K3/26Carbonates; Bicarbonates
    • C08K2003/265Calcium, strontium or barium carbonate

Abstract

A pasty organic peroxide cross-linking agent belongs to the technical field of peroxide cross-linking agents, and particularly relates to a pasty organic peroxide cross-linking agent and a compounding process thereof. The paint is characterized by comprising the following components in parts by weight: 47-53% of dibenzoyl peroxide, 14-18% of water, 0.1-2.0% of nonionic surfactant, 20-26% of desensitizer and 4-15% of inorganic filler. The invention has the advantages of uniform product, no layering, convenient transportation and use, safety and reliability.

Description

Pasty organic peroxide crosslinking agent and compounding process thereof
Technical Field
The invention belongs to the technical field of peroxide crosslinking agents, and particularly relates to a paste organic peroxide crosslinking agent and a compounding process thereof.
Background
The high-purity organic peroxide is extremely sensitive to heat, vibration, impact, friction and the like, is extremely easy to decompose, can generate a large amount of gases such as methane, ethane, acetone, carbon dioxide and the like, and the generated gases form pressure which is enough to damage a packaging material in a closed packaging material, so that explosion and fire disasters are extremely easy to generate. In order to ensure the safety of the organic peroxide in use and storage, auxiliary materials such as desensitizers, stabilizers and the like are usually added into the high-purity organic peroxide to prepare a mixture with stable properties and uniform texture. Water is the most common and cheap desensitizer, but after high-purity organic peroxide is dispersed in water, the phenomena of system instability such as sedimentation, floating and the like often occur, so that the uniformity of a product is poor, and the use of the product is influenced. Meanwhile, high-purity organic peroxide is simply dispersed in water, and the subsequent reaction system is usually in an organic environment, so that the problem of uneven dispersion is easily caused during use. And when the environmental temperature is lower than 0 ℃, water is easy to freeze, so that the relative concentration of the high-purity organic peroxide is increased, and the danger is increased.
Disclosure of Invention
The invention aims to provide a pasty organic peroxide cross-linking agent and a compounding process thereof, so as to achieve the purposes of uniform product, no layering, convenient transportation and use, safety and reliability.
The invention provides a pasty organic peroxide cross-linking agent which is characterized by comprising the following components in parts by weight: 47-53% of dibenzoyl peroxide, 14-18% of water, 0.1-2.0% of nonionic surfactant, 20-26% of desensitizer and 4-15% of inorganic filler.
Further, the nonionic surfactant refers to polyether nonionic surfactant, and is a block polymer of ethylene oxide and propylene oxide.
Further, the desensitizer refers to any one or more of oligomeric isobutylene, tributyl citrate and acetyl tributyl citrate.
Further, the polymerization degree range of the oligomeric isobutylene is 450-3000.
Further, the inorganic filler is one or more of calcium carbonate, silicon dioxide, attapulgite and clay, and the particle size of the inorganic filler is less than or equal to 2 mu m.
Further, the compounding process of the paste organic peroxide crosslinking agent comprises the following steps:
step 1, uniformly mixing dibenzoyl peroxide and water according to the proportion of 47-53 percent of dibenzoyl peroxide and 14-18 percent of water by weight to prepare a mixture of dibenzoyl peroxide and water for later use;
step 2, adding 20-26% of desensitizer into the mixture of the dibenzoyl peroxide and the water in the step 1 by weight, and uniformly stirring to prepare a mixture of the dibenzoyl peroxide, the water and the desensitizer for later use;
and 3, adding 0.1-2.0% of nonionic surfactant and 4-15% of inorganic filler by weight into the mixture of the dibenzoyl peroxide, the water and the desensitizer in the step 2, and emulsifying to obtain the pasty organic peroxide crosslinking agent.
Further, the compounding process of the paste organic peroxide crosslinking agent comprises the following steps:
step 1, uniformly mixing dibenzoyl peroxide and water according to the proportion of 47-53 percent of dibenzoyl peroxide and 14-18 percent of water by weight to prepare a mixture of dibenzoyl peroxide and water for later use;
step 2, adding 20-24% of desensitizer by weight into the mixture of the dibenzoyl peroxide and the water in the step 1, and uniformly stirring to prepare a mixture of the dibenzoyl peroxide, the water and the desensitizer for later use;
and 3, adding 0.1-2.0% of nonionic surfactant and 4-15% of inorganic filler by weight into the mixture of the dibenzoyl peroxide, the water and the desensitizer in the step 2, and emulsifying to obtain the pasty organic peroxide crosslinking agent.
And 4, supplementing a desensitizer into the emulsion obtained in the step 3 by weight, so that the desensitizer is added by 20-26% by weight, and continuously emulsifying for 1.0-2.0 h to obtain the pasty organic peroxide crosslinking agent.
Further, the step 2 of uniformly stirring is to start a stirring device, stir for 0.5 to 1.0 hour at a rotation speed of 2000 to 2500r/min, and uniformly stir.
Further, the emulsification in the step 3 is to start an emulsifying machine for emulsification, and the emulsification is continuously performed for 1.0h to 3.0 h.
Further, during the compounding, a temperature control device is started, and the temperature of the system is always kept at 20-25 ℃.
The invention provides a pasty organic peroxide cross-linking agent and a compounding process thereof, and the innovation points and the beneficial effects are mainly embodied in the following aspects:
1. the desensitizer and the inorganic filler ensure that the pasty organic peroxide crosslinking agent obtained by compounding has uniform texture;
2. the non-ionic surfactant ensures that the compounded pasty organic peroxide cross-linking agent has excellent physical stability and does not have the unstable phenomena of sedimentation, floating and the like;
3. the particle size of the inorganic filler is less than or equal to 2 mu m, so that the pasty organic peroxide crosslinking agent has good fineness and physical stability, and is not easy to delaminate;
4. the process mixes dibenzoyl peroxide and water in advance, the dibenzoyl peroxide content is 73-76% (by weight), the rest is water, the organic peroxide raw material is dibenzoyl peroxide with the water content of 24-27%, and the process is safer compared with dry dibenzoyl peroxide.
The pasty organic peroxide crosslinking agent prepared by the preparation process provided by the invention has the advantages that the physical form is pasty, the physical stability is excellent, the product is placed for 12 months or more after standing, and the product is uniform and has no layering. Therefore, the invention has the advantages of uniform product, no layering, convenient transportation and use, safety and reliability.
Detailed Description
The invention is further illustrated by the following examples. The product physical stability of the product index is as follows: standing the product for 12 months or more, wherein the product is uniform and has no layering, and the product is excellent; the product is kept stand for 6 months or more, is uniform and has no layering, and is good; standing the product for 3 months or more, wherein the product is uniform and has no layering, and the product is medium; the product is not uniform and layered when the standing time of the product is less than 3 months.
Example 1:
a compounding process of a paste organic peroxide crosslinking agent comprises the following steps:
step 1, uniformly mixing dibenzoyl peroxide and water according to the proportion of 47-53 percent of dibenzoyl peroxide and 14-18 percent of water by weight to prepare a mixture of dibenzoyl peroxide and water for later use;
step 2, adding 20-24% of desensitizer into the mixture of the dibenzoyl peroxide and the water in the step 1 by weight, starting a stirring device, stirring for 0.5-1.0 h at a rotating speed of 2000-2500 r/min, and uniformly stirring to prepare a mixture of the dibenzoyl peroxide, the water and the desensitizer for later use;
step 3, adding 0.1-2.0% of nonionic surfactant and 4-15% of inorganic filler by weight into the mixture of the dibenzoyl peroxide, the water and the desensitizer in the step 2, starting an emulsifying machine for emulsification, and continuously performing the emulsification for 1.0-3.0 hours to prepare an emulsion;
and 4, supplementing a desensitizer into the emulsion obtained in the step 3 by weight, so that the desensitizer is added by 20-26% by weight, and continuously emulsifying for 1.0-2.0 h to obtain the pasty organic peroxide crosslinking agent.
During compounding, the temperature control device is started to always maintain the system temperature at 20-25 ℃.
The nonionic surfactant is polyether nonionic surfactant, and is a block polymer of methyl ethylene oxide and ethylene oxide.
The desensitizer is any one or more of oligomeric isobutylene, tributyl citrate and acetyl tributyl citrate, and the polymerization degree of the oligomeric isobutylene ranges from 450 to 3000.
The inorganic filler is one or more of calcium carbonate, silicon dioxide, attapulgite and clay, and the particle size of the inorganic filler is less than or equal to 2 μm.
Example 2:
a compounding process of a paste organic peroxide crosslinking agent comprises the following steps:
step 1, uniformly mixing dibenzoyl peroxide and water according to the proportion of 47-53 percent of dibenzoyl peroxide and 14-18 percent of water by weight to prepare a mixture of dibenzoyl peroxide and water for later use;
step 2, adding 20-26% of desensitizer into the mixture of the dibenzoyl peroxide and the water in the step 1 by weight, and uniformly stirring to prepare a mixture of the dibenzoyl peroxide, the water and the desensitizer for later use;
and 3, adding 0.1-2.0% of nonionic surfactant and 4-15% of inorganic filler by weight into the mixture of the dibenzoyl peroxide, the water and the desensitizer in the step 2, and emulsifying to obtain the pasty organic peroxide crosslinking agent.
During compounding, the temperature control device is started to always maintain the system temperature at 20-25 ℃.
The nonionic surfactant is polyether nonionic surfactant, and is a block polymer of methyl ethylene oxide and ethylene oxide.
The desensitizer is any one or more of oligomeric isobutylene, tributyl citrate and acetyl tributyl citrate, and the polymerization degree of the oligomeric isobutylene ranges from 450 to 3000.
The inorganic filler is one or more of calcium carbonate, silicon dioxide, attapulgite and clay, and the particle size of the inorganic filler is less than or equal to 2 μm.
Example 3:
a compounding process of a paste organic peroxide crosslinking agent comprises the following steps:
step 1, dibenzoyl peroxide and water are mixed in advance, wherein the content of the dibenzoyl peroxide is 75 percent (by weight), and the rest is water, so as to prepare a mixture of the dibenzoyl peroxide and the water for later use;
step 2, adding 2680g of dibenzoyl peroxide and water mixture (with the water content of 25%) and 920g of acetyl tributyl citrate obtained in the step 1 into a 5L enamel reaction kettle provided with a common emulsifying machine and a stirrer, starting a stirring device, stirring for 0.6h at the rotating speed of 2200r/min, and uniformly stirring to obtain a mixture of dibenzoyl peroxide, water and acetyl tributyl citrate for later use;
step 3, adding 80g of polyether type nonionic surfactant Pluronic RPE and 240g of nano calcium carbonate into the mixture of the dibenzoyl peroxide, the water and the acetyl tributyl citrate obtained in the step 2 by weight, starting an emulsifying machine to emulsify for 2.0 hours continuously to obtain an emulsion;
and 4, additionally adding 80g of oligomeric isobutylene into the emulsion obtained in the step 3 by weight, and continuing to emulsify for 1.2h to obtain the pasty organic peroxide crosslinking agent.
The polyether nonionic surfactant Pluronic RPE is a block polymer of methyl ethylene oxide and ethylene oxide.
The polymerization degree of the reduced polyisobutylene is 600.
The particle size of the nano calcium carbonate is 1 mu m.
During the compounding, the temperature control device is started, and the system temperature is always kept at 22 ℃. The inspection results of the prepared paste organic peroxide crosslinking agent are as follows:
item Results Analytical method
Physical form Paste form Visual inspection of
Peroxide content 51.0% Iodometry
Active oxygen 3.37% Iodometry
Viscosity (hake viscosity 20 ℃ C.) 47Pas Rotary viscometer
Density of 1.18g/cm3 Densimeter
Physical stability Superior food Visual inspection of
Example 4:
a compounding process of a paste organic peroxide crosslinking agent comprises the following steps:
step 1, dibenzoyl peroxide and water are mixed in advance, wherein the dibenzoyl peroxide content is 76% (by weight), and the balance is water, so as to prepare a mixture of the dibenzoyl peroxide and the water for later use;
step 2, adding 2520g of the mixture (with the water content of 24%) of dibenzoyl peroxide and water and 1040g of tributyl citrate obtained in the step 1 into a 5L enamel reaction kettle provided with a common emulsifying machine and a stirrer, starting a stirring device, stirring for 0.7h at the rotation speed of 2300r/min, and uniformly stirring to obtain a mixture of dibenzoyl peroxide, water and tributyl citrate for later use;
and 3, adding 40g of polyether nonionic surfactant Pluronic RPE and 400g of nano calcium carbonate into the mixture of the dibenzoyl peroxide, the water and the tributyl citrate obtained in the step 2 by weight, starting an emulsifying machine to emulsify for 1.5 hours, and obtaining the pasty organic peroxide cross-linking agent.
The polyether nonionic surfactant Pluronic RPE is a block polymer of methyl ethylene oxide and ethylene oxide.
The particle size of the nano calcium carbonate is 2 mu m.
During the compounding, the temperature control device is started, and the system temperature is always kept at 24 ℃. The inspection results of the prepared paste organic peroxide crosslinking agent are as follows:
item Results Analytical method
Physical form Paste form Visual inspection of
Peroxide content 47.0% Iodometry
Active oxygen 3.10% Iodometry
Viscosity (hake viscosity 20 ℃ C.) 50Pas Rotary viscometer
Density of 1.21g/cm3 Densimeter
Physical stability Superior food Visual inspection of
Example 5:
a compounding process of a paste organic peroxide crosslinking agent comprises the following steps:
step 1, dibenzoyl peroxide and water are mixed in advance, the dibenzoyl peroxide content is 73% (by weight), and the rest is water, so as to prepare a mixture of the dibenzoyl peroxide and the water for later use;
step 2, adding 2840g of dibenzoyl peroxide and water mixture (the water content is 27%) and 800g of tributyl citrate obtained in the step 1 into a 5L enamel reaction kettle provided with a common emulsifying machine and a stirrer, starting a stirring device, stirring for 0.8h at the rotation speed of 2300r/min, and uniformly stirring to obtain a mixture of dibenzoyl peroxide, water and tributyl citrate for later use;
step 3, adding 80g of polyether type nonionic surfactant Pluronic RPE and 160g of nano calcium carbonate into the mixture of the dibenzoyl peroxide, the water and the tributyl citrate obtained in the step 2 by weight, starting an emulsifying machine to emulsify for 2.5 hours continuously to obtain an emulsion;
and 4, additionally adding 120g of oligomeric isobutylene into the emulsion obtained in the step 3 by weight, and continuing to emulsify for 1.6h to obtain the pasty organic peroxide crosslinking agent.
The polyether nonionic surfactant Pluronic RPE is a block polymer of methyl ethylene oxide and ethylene oxide.
The polymerization degree of the reduced polyisobutylene is 1800.
The particle size of the nano calcium carbonate is 1 mu m.
The polyether nonionic surfactant Pluronic RPE is a block polymer of methyl ethylene oxide and ethylene oxide.
During the compounding, the temperature control device is started, and the system temperature is always kept at 23 ℃. The inspection results of the prepared paste organic peroxide crosslinking agent are as follows:
item Results Analytical method
Physical form Paste form Visual inspection of
Peroxide content 53.0% Iodometry
Active oxygen 3.50% Iodometry
Viscosity (hake viscosity 20 ℃ C.) 49Pas Rotary viscometer
Density of 1.19g/cm3 Densimeter
Physical stability Superior food Visual inspection of
Example 6:
a compounding process of a paste organic peroxide crosslinking agent comprises the following steps:
step 1, dibenzoyl peroxide and water are mixed in advance, wherein the dibenzoyl peroxide content is 74 percent (by weight), and the balance is water, so as to prepare a mixture of the dibenzoyl peroxide and the water for later use;
step 2, adding 2720g of dibenzoyl peroxide and water mixture (the water content is 26%) and 800g of acetyl tributyl citrate obtained in the step 1 into a 5L enamel reaction kettle provided with a common emulsifying machine and a stirrer, starting a stirring device, stirring for 0.9h at the rotation speed of 2300r/min, and uniformly stirring to obtain a mixture of dibenzoyl peroxide, water and acetyl tributyl citrate for later use;
and 3, adding 4g of polyether type nonionic surfactant Pluronic RPE and 476g of precipitation method silicon dioxide into the mixture of the dibenzoyl peroxide, the water and the acetyl tributyl citrate in the step 2 by weight, starting an emulsifying machine to emulsify for 1.8 hours, and preparing the pasty organic peroxide crosslinking agent.
The polyether nonionic surfactant Pluronic RPE is a block polymer of methyl ethylene oxide and ethylene oxide.
The particle diameter of the silica is 1 to 2 μm.
During the compounding, the temperature control device is started, and the system temperature is always kept at 23 ℃. The inspection results of the prepared paste organic peroxide crosslinking agent are as follows:
item Results Analytical method
Physical form Paste form Visual inspection of
Peroxide content 51.0% Iodometry
Active oxygen 3.30% Iodometry
Viscosity (hake viscosity 20 ℃ C.) 50Pas Rotary viscometer
Density of 1.18g/cm3 Densimeter
Physical stability Superior food Visual inspection of
Example 7:
a paste-like organic peroxide-based crosslinking agent comprising the following components by weight: 48 to 52 percent of dibenzoyl peroxide, 15 to 17 percent of water, 0.16 percent of nonionic surfactant, 21 to 25 percent of desensitizer and 5 to 14 percent of inorganic filler. The nonionic surfactant refers to polyether nonionic surfactant, and is a block polymer of methyl ethylene oxide and ethylene oxide. The desensitizer refers to any one or more of oligomeric isobutylene, tributyl citrate and acetyl tributyl citrate. The polymerization degree range of the oligomeric isobutylene is 500-2500. The inorganic filler is one or more of calcium carbonate, silicon dioxide, attapulgite and clay, and the particle size of the inorganic filler is 1-2 mu m.
Example 8:
a paste-like organic peroxide-based crosslinking agent comprising the following components by weight: 49-51% of dibenzoyl peroxide, 14-16% of water, 0.15% of nonionic surfactant, 22-24% of desensitizer and 6-12% of inorganic filler. The nonionic surfactant refers to polyether nonionic surfactant, and is a block polymer of methyl ethylene oxide and ethylene oxide. The desensitizer refers to any one or more of oligomeric isobutylene, tributyl citrate and acetyl tributyl citrate. The polymerization degree range of the oligomeric isobutylene is 1200-2000. The inorganic filler is one or more of calcium carbonate, silicon dioxide, attapulgite and clay, and the particle size of the inorganic filler is 2 μm.
Example 9:
a paste-like organic peroxide-based crosslinking agent comprising the following components by weight: 50% of dibenzoyl peroxide, 16.6% of water, 0.12% of nonionic surfactant, 23% of desensitizer and 7% -9% of inorganic filler. The nonionic surfactant refers to polyether nonionic surfactant, and is a block polymer of methyl ethylene oxide and ethylene oxide. The desensitizer refers to any one or more of oligomeric isobutylene, tributyl citrate and acetyl tributyl citrate. The degree of polymerization of the oligomeric isobutene ranged from 2600. The inorganic filler is one or more of calcium carbonate, silicon dioxide, attapulgite and clay, and the particle size of the inorganic filler is 1 μm.
The pasty organic peroxide crosslinking agent and the preparation process thereof provided by the invention can be used as a crosslinking agent of ethylene propylene rubber, ethylene propylene diene monomer rubber and silicon rubber, and can also be used as a crosslinking agent and a curing agent of unsaturated resin or analogues thereof.

Claims (10)

1. A paste-like organic peroxide-based crosslinking agent, characterized by comprising the following components by weight: 47-53% of dibenzoyl peroxide, 14-18% of water, 0.1-2.0% of nonionic surfactant, 20-26% of desensitizer and 4-15% of inorganic filler.
2. The paste-like organic peroxide-based crosslinking agent according to claim 1, wherein the nonionic surfactant is a polyether-type nonionic surfactant and is a block polymer of methyl ethylene oxide and ethylene oxide.
3. The paste-like organic peroxide-based crosslinking agent according to claim 1, wherein the phlegmatizer is any one or more of oligomeric isobutylene, tributyl citrate, and acetyl tributyl citrate.
4. The paste-like organic peroxide-based crosslinking agent according to claim 3, wherein the degree of polymerization of the oligomeric isobutylene is in the range of 450 to 3000.
5. The paste-like organic peroxide-based crosslinking agent according to claim 1, wherein the inorganic filler is one or more selected from the group consisting of calcium carbonate, silica, attapulgite and clay, and the particle size of the inorganic filler is 2 μm or less.
6. The compounding process of the paste organic peroxide crosslinking agent according to claim 1, comprising the steps of:
step 1, uniformly mixing dibenzoyl peroxide and water according to the proportion of 47-53 percent of dibenzoyl peroxide and 14-18 percent of water by weight to prepare a mixture of dibenzoyl peroxide and water for later use;
step 2, adding 20-26% of desensitizer into the mixture of the dibenzoyl peroxide and the water in the step 1 by weight, and uniformly stirring to prepare a mixture of the dibenzoyl peroxide, the water and the desensitizer for later use;
and 3, adding 0.1-2.0% of nonionic surfactant and 4-15% of inorganic filler by weight into the mixture of the dibenzoyl peroxide, the water and the desensitizer in the step 2, and emulsifying to obtain the pasty organic peroxide crosslinking agent.
7. The compounding process of the paste organic peroxide crosslinking agent according to claim 1, comprising the steps of:
step 1, uniformly mixing dibenzoyl peroxide and water according to the proportion of 47-53 percent of dibenzoyl peroxide and 14-18 percent of water by weight to prepare a mixture of dibenzoyl peroxide and water for later use;
step 2, adding 20-24% of desensitizer by weight into the mixture of the dibenzoyl peroxide and the water in the step 1, and uniformly stirring to prepare a mixture of the dibenzoyl peroxide, the water and the desensitizer for later use;
step 3, adding 0.1-2.0% of nonionic surfactant and 4-15% of inorganic filler by weight into the mixture of the dibenzoyl peroxide, the water and the desensitizer in the step 2, and emulsifying to obtain an emulsion;
and 4, supplementing a desensitizer into the emulsion obtained in the step 3 by weight, so that the desensitizer is added by 20-26% by weight, and continuously emulsifying for 1.0-2.0 h to obtain the pasty organic peroxide crosslinking agent.
8. The process of claim 6 or 7, wherein the step 2 of uniformly stirring is to start a stirring device, stir at a rotation speed of 2000 r/min-2500 r/min for 0.5 h-1.0 h, and uniformly stir.
9. The process of claim 6 or 7, wherein the step 3 of emulsifying comprises starting an emulsifying machine for emulsifying for 1.0-3.0 h.
10. The process according to claim 6 or 7, wherein the temperature control device is turned on to maintain the temperature of the system at 20-25 ℃ during the compounding.
CN202011425730.8A 2020-12-09 2020-12-09 Pasty organic peroxide crosslinking agent and compounding process thereof Pending CN112521658A (en)

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Application publication date: 20210319