阅读说明：本技术 一种环保型氯磺化聚乙烯橡胶的制备方法 (Preparation method of environment-friendly chlorosulfonated polyethylene rubber ) 是由 吴彤 石楠 张泽宇 于 2019-04-09 设计创作，主要内容包括：环保型氯磺化聚乙烯橡胶的制备方法,步骤(1)按配比称取氯磺化聚乙烯、补强填充剂、二辛脂、环氧树脂、硬脂酸钠、顺丁橡胶、丁苯橡胶、季戊四醇、TOTM油、环保型增塑剂、增粘树脂、AW防老剂送入密炼机中混炼；步骤(2)称取纳米硅酸盐、氧化镁、轻质碳酸钙、白炭黑加入研磨机研磨；步骤(3)将偶联剂、脱模剂、FL流动助剂、所述混合粉末与步骤(1)得到的混合物料加入开炼机中混炼；步骤(4)加入DM促进剂、DPTT促进剂、HVA-2促进剂混炼,得环保型氯磺化聚乙烯橡胶。本发明提供的环保型氯磺化聚乙烯橡胶采用环保型增塑剂和不含铅的环保型硫化促进剂,绿色环保；具有优异的耐热性能、耐介质性能、耐油及耐燃性能。(The preparation method of environment-friendly chlorosulfonated polyethylene rubber comprises the following steps of (1) weighing chlorosulfonated polyethylene, a reinforcing filler, dioctyl ester, epoxy resin, sodium stearate, butadiene rubber, styrene butadiene rubber, pentaerythritol, TOTM oil, an environment-friendly plasticizer, tackifying resin and an AW anti-aging agent according to a ratio, and feeding the materials into an internal mixer for mixing; weighing nano silicate, magnesium oxide, light calcium carbonate and white carbon black, adding into a grinding machine, and grinding; step (3) adding a coupling agent, a release agent, a FL flow aid, the mixed powder and the mixed material obtained in the step (1) into an open mill for mixing; and (4) adding a DM accelerator, a DPTT accelerator and an HVA-2 accelerator, and mixing to obtain the environment-friendly chlorosulfonated polyethylene rubber. The environment-friendly chlorosulfonated polyethylene rubber provided by the invention adopts an environment-friendly plasticizer and a lead-free environment-friendly vulcanization accelerator, and is environment-friendly; has excellent heat resistance, medium resistance, oil resistance and flame resistance.)

1. The preparation method of the environment-friendly chlorosulfonated polyethylene rubber is characterized by comprising the following components in parts by weight: 90-110 parts of chlorosulfonated polyethylene, 25-60 parts of reinforcing filler, 20-40 parts of nano silicate, 10-30 parts of white carbon black, 10-35 parts of light calcium carbonate, 5-20 parts of dioctyl phthalate, 5-20 parts of epoxy resin, 1-2 parts of sodium stearate, 3-5 parts of butadiene rubber, 2-6 parts of styrene butadiene rubber, 2-4 parts of pentaerythritol, 5-10 parts of TOTM oil, 2-3 parts of coupling agent, 2-3 parts of mold release agent, 5-20 parts of environment-friendly plasticizer, 0.5-4 parts of tackifying resin, 1-3 parts of AW anti-aging agent, 5-15 parts of magnesium oxide, 1-4 parts of FL flow promoter, 0.5-2.5 parts of DM accelerator, 0.5-2.5 parts of DPTT accelerator and 0.5-2.5 parts of HVA-2 accelerator;

the preparation method of the environment-friendly chlorosulfonated polyethylene rubber comprises the following steps:

weighing chlorosulfonated polyethylene, a reinforcing filler, dioctyl phthalate, epoxy resin, sodium stearate, butadiene rubber, styrene-butadiene rubber, pentaerythritol, TOTM oil, an environment-friendly plasticizer, tackifying resin and an AW (ethylene-propylene-diene monomer) antioxidant according to a ratio, and feeding the materials into an internal mixer for mixing for 8-12min at the mixing temperature of 65-75 ℃;

weighing nano silicate, magnesium oxide, light calcium carbonate and white carbon black, adding into a grinding machine, and grinding for 20-30min at a speed of 80-120r/min to obtain mixed powder;

step (3) adding a coupling agent, a release agent, a FL flow aid, the mixed powder and the mixed material obtained in the step (1) into an open mill, and completely mixing, wherein the mixing temperature is 75-85 ℃, and the mixing time is 3-4 min;

and (4) heating to 88-93 ℃, adding a DM accelerator, a DPTT accelerator and an HVA-2 accelerator, mixing for 1-3min, and cooling to 15-35 ℃ in a ventilating manner to obtain the environment-friendly chlorosulfonated polyethylene rubber.

2. The preparation method of the environment-friendly chlorosulfonated polyethylene rubber according to claim 1, which is characterized by comprising the following components in parts by weight: 90 parts of chlorosulfonated polyethylene, 25 parts of reinforcing filler, 20 parts of nano silicate, 10 parts of white carbon black, 10 parts of light calcium carbonate, 5 parts of dioctyl ester, 5 parts of epoxy resin, 1 part of sodium stearate, 3-5 parts of butadiene rubber, 2 parts of styrene butadiene rubber, 2 parts of pentaerythritol, 5 parts of TOTM oil, 2 parts of coupling agent, 2 parts of release agent, 5 parts of environment-friendly plasticizer, 0.5 part of tackifying resin, 1 part of AW anti-aging agent, 5 parts of magnesium oxide, 1 part of FL flow promoter, 0.5 part of DM promoter, 0.5 part of DPTT promoter and 0.5 part of HVA-2 promoter.

3. The preparation method of the environment-friendly chlorosulfonated polyethylene rubber according to claim 1, which is characterized by comprising the following components in parts by weight: 110 parts of chlorosulfonated polyethylene, 60 parts of reinforcing filler, 40 parts of nano silicate, 30 parts of white carbon black, 35 parts of light calcium carbonate, 20 parts of dioctyl ester, 20 parts of epoxy resin, 2 parts of sodium stearate, 5 parts of butadiene rubber, 6 parts of styrene butadiene rubber, 4 parts of pentaerythritol, 10 parts of TOTM oil, 3 parts of coupling agent, 3 parts of mold release agent, 20 parts of environment-friendly plasticizer, 4 parts of tackifying resin, 3 parts of AW anti-aging agent, 15 parts of magnesium oxide, 4 parts of FL flow promoter, 2.5 parts of DM promoter, 2.5 parts of DPTT promoter and 2.5 parts of HVA-2 promoter.

4. The preparation method of the environment-friendly chlorosulfonated polyethylene rubber according to claim 1, which is characterized by comprising the following components in parts by weight: 100 parts of chlorosulfonated polyethylene, 40 parts of reinforcing filler, 30 parts of nano silicate, 20 parts of white carbon black, 22 parts of light calcium carbonate, 12 parts of dioctyl ester, 12 parts of epoxy resin, 2 parts of sodium stearate, 3 parts of butadiene rubber, 4 parts of styrene butadiene rubber, 3 parts of pentaerythritol, 7 parts of TOTM oil, 2 parts of coupling agent, 3 parts of release agent, 12 parts of environment-friendly plasticizer, 2 parts of tackifying resin, 2 parts of AW anti-aging agent, 10 parts of magnesium oxide, 2 parts of FL flow promoter, 1 part of DM promoter, 1 part of DPTT promoter and 1 part of HVA-2 promoter.

5. The method for preparing environment-friendly chlorosulfonated polyethylene rubber according to claim 1, wherein the chlorosulfonated polyethylene has a volatile content of not more than 1%, a chlorine content of 33 to 37%, a sulfur content of 0.8 to 1.2%, and a Mooney viscosity of 40 to 60.

6. The method for preparing environment-friendly chlorosulfonated polyethylene rubber according to claim 1, wherein the epoxy resin is E51 epoxy resin, the epoxy equivalent weight is 175-210, and the epoxy value is 0.48-0.51.

7. The method for preparing environment-friendly chlorosulfonated polyethylene rubber according to claim 1, wherein the dioctyl ester is one of dioctyl phthalate, dioctyl adipate or dioctyl azelate.

8. The method for preparing environment-friendly chlorosulfonated polyethylene rubber according to claim 1, wherein methyl silicone oil is used as the mold release agent.

9. The method for preparing environment-friendly chlorosulfonated polyethylene rubber according to claim 1, wherein an environment-friendly plasticizer TP-95 is used as the environment-friendly plasticizer.

10. The method for preparing environment-friendly chlorosulfonated polyethylene rubber according to claim 1, wherein 2402 phenolic resin is used as the tackifying resin.

Technical Field

The invention relates to chlorosulfonated polyethylene rubber, in particular to a preparation method of environment-friendly chlorosulfonated polyethylene rubber.

Background

In recent years, with the rapid development of the automobile industry, the requirements of automobile rubber pipes on rubber materials are higher and higher, and chlorosulfonated polyethylene rubber (CSM) materials are widely applied to automobile connecting rubber pipes such as automobile air vent rubber pipes due to good heat resistance, aging resistance, flame resistance and medium resistance. In the whole vehicle design process, the light weight, compactness and reasonable layout of the vehicle are considered, and parts cannot interfere with each other. The whole vehicle is designed with a plurality of parts made of large and small metals, the space shape and the trend are difficult to bend freely, the rubber hose plays an important role, and the defects of mutual friction, mutual interference, difficult bending, poor sealing performance of an interface of a butt joint part and the like between a metal part and a metal hard pipe are overcome.

With the enhancement of environmental awareness, the requirements on the safety and environmental protection of the used rubber materials are higher and higher. At present, most of chlorosulfonated polyethylene rubber commonly used in China adopts lead-containing metal oxide, and although the lead-containing metal oxide can achieve good thermal aging resistance due to good crosslinking degree, the lead-containing metal oxide is volatilized in a hot environment for a long time and seriously harms the life safety of people. And environmental protection provisions made globally are mainly concerned with the use of: mercury, lead, chromium, cadmium, etc. (ROSH), and it is therefore of great importance to develop a formulation that does not contain harmful metal oxides.

Disclosure of Invention

In order to solve the problems in the prior art, the invention provides a preparation method of environment-friendly chlorosulfonated polyethylene rubber, which can replace a chlorosulfonated polyethylene formula containing harmful metal oxides. The environmental-friendly chlorosulfonated polyethylene rubber formula can meet the performance requirements, and the used materials are environment-friendly and safe to human bodies.

The technical scheme adopted by the invention for solving the technical problems is as follows: the preparation method of the environment-friendly chlorosulfonated polyethylene rubber comprises the following components in parts by weight: 90-110 parts of chlorosulfonated polyethylene, 25-60 parts of reinforcing filler, 20-40 parts of nano silicate, 10-30 parts of white carbon black, 10-35 parts of light calcium carbonate, 5-20 parts of dioctyl ester, 5-20 parts of epoxy resin, 1-2 parts of sodium stearate, 3-5 parts of butadiene rubber, 2-6 parts of styrene butadiene rubber, 2-4 parts of pentaerythritol, 5-10 parts of TOTM oil, 2-3 parts of coupling agent, 2-3 parts of release agent, 5-20 parts of environment-friendly plasticizer, 0.5-4 parts of tackifying resin, 1-3 parts of AW anti-aging agent, 5-15 parts of magnesium oxide, 1-4 parts of FL flow promoter, 0.5-2.5 parts of DM accelerator, 0.5-2.5 parts of DPTT accelerator and 0.5-2.5 parts of HVA-2 accelerator.

The preparation method of the environment-friendly chlorosulfonated polyethylene rubber comprises the following steps:

weighing chlorosulfonated polyethylene, a reinforcing filler, dioctyl phthalate, epoxy resin, sodium stearate, butadiene rubber, styrene-butadiene rubber, pentaerythritol, TOTM oil, an environment-friendly plasticizer, tackifying resin and an AW (ethylene-propylene-diene monomer) antioxidant according to a ratio, and feeding the materials into an internal mixer for mixing for 8-12min at the mixing temperature of 65-75 ℃;

weighing nano silicate, magnesium oxide, light calcium carbonate and white carbon black, adding into a grinding machine, and grinding for 20-30min at a speed of 80-120r/min to obtain mixed powder;

step (3) adding the coupling agent, the release agent, the FL flow promoter, the mixed powder and the mixed material obtained in the step (1) into an open mill for complete mixing, wherein the mixing temperature is 75-85 ℃, and the mixing time is 3-4 min;

and (4) heating to 88-93 ℃, adding a DM accelerator, a DPTT accelerator and an HVA-2 accelerator, mixing for 1-3min, and cooling to 15-35 ℃ in a ventilating manner to obtain the environment-friendly chlorosulfonated polyethylene rubber.

Compared with the prior art, the invention has the advantages that:

(1) the environment-friendly chlorosulfonated polyethylene rubber provided by the invention solves the problem that the conventional formula is easy to cause scorching and harm and pollution to personnel, equipment and environment. Firstly, chlorosulfonated polyethylene, a reinforcing filler, dioctyl ester, epoxy resin, sodium stearate, butadiene rubber, styrene butadiene rubber, pentaerythritol, TOTM oil, an environment-friendly plasticizer, tackifying resin and an AW (ethylene diamine tetra butyl) antioxidant are fed into an internal mixer to be mixed, and then a coupling agent, a release agent and an FL flow aid are added to be mixed in an open mill, so that drying treatment of all materials is not needed, and the production cost is saved. The anti-aging agent can reduce the cost, improve the adhesiveness and the like, and improve the processing performance.

(2) The environment-friendly chlorosulfonated polyethylene rubber provided by the invention is added with the release agent and the magnesium oxide, so that the smoothness and cleanliness of the chlorosulfonated polyethylene surface of the rubber are improved, the chlorosulfonated polyethylene surface is easy to separate, smooth and clean, and the magnesium oxide can effectively absorb byproducts such as hydrogen chloride and the like.

(3) The environment-friendly chlorosulfonated polyethylene rubber provided by the invention adopts an environment-friendly plasticizer and a lead-free environment-friendly vulcanization accelerator, and is environment-friendly; has excellent heat resistance, medium resistance, oil resistance and flame resistance.

Additional aspects and advantages of the invention will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the invention.

Drawings

In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.

FIG. 1 is a schematic flow chart of the preparation method of the present invention.

Detailed Description

Exemplary embodiments of the present disclosure will be described in more detail below with reference to the accompanying drawings, in order that the present disclosure may be more fully understood and fully conveyed to those skilled in the art. While the exemplary embodiments of the present disclosure are shown in the drawings, it should be understood that the invention is not limited to the embodiments set forth herein.

The preparation method of the environment-friendly chlorosulfonated polyethylene rubber comprises the following components in parts by weight: 90-110 parts of chlorosulfonated polyethylene, 25-60 parts of reinforcing filler, 20-40 parts of nano silicate, 10-30 parts of white carbon black, 10-35 parts of light calcium carbonate, 5-20 parts of dioctyl ester, 5-20 parts of epoxy resin, 1-2 parts of sodium stearate, 3-5 parts of butadiene rubber, 2-6 parts of styrene butadiene rubber, 2-4 parts of pentaerythritol, 5-10 parts of TOTM oil, 2-3 parts of coupling agent, 2-3 parts of release agent, 5-20 parts of environment-friendly plasticizer, 0.5-4 parts of tackifying resin, 1-3 parts of AW anti-aging agent, 5-15 parts of magnesium oxide, 1-4 parts of FL flow promoter, 0.5-2.5 parts of DM accelerator, 0.5-2.5 parts of DPTT accelerator and 0.5-2.5 parts of HVA-2 accelerator.

The preparation method of the environment-friendly chlorosulfonated polyethylene rubber comprises the following steps:

weighing chlorosulfonated polyethylene, a reinforcing filler, dioctyl phthalate, epoxy resin, sodium stearate, butadiene rubber, styrene-butadiene rubber, pentaerythritol, TOTM oil, an environment-friendly plasticizer, tackifying resin and an AW (ethylene-propylene-diene monomer) antioxidant according to a ratio, and feeding the materials into an internal mixer for mixing for 8-12min at the mixing temperature of 65-75 ℃;

weighing nano silicate, magnesium oxide, light calcium carbonate and white carbon black, adding into a grinding machine, and grinding for 20-30min at a speed of 80-120r/min to obtain mixed powder;

step (3) adding the coupling agent, the release agent, the FL flow promoter, the mixed powder and the mixed material obtained in the step (1) into an open mill for complete mixing, wherein the mixing temperature is 75-85 ℃, and the mixing time is 3-4 min;

and (4) heating to 88-93 ℃, adding a DM accelerator, a DPTT accelerator and an HVA-2 accelerator, mixing for 1-3min, and cooling to 15-35 ℃ in a ventilating manner to obtain the environment-friendly chlorosulfonated polyethylene rubber.

Specifically optimized, the chlorosulfonated polyethylene has the volatile component of less than or equal to 1 percent, the chlorine content of 33-37 percent, the sulfur content of 0.8-1.2 percent and the Mooney viscosity of 40-60 percent.

Specifically, the epoxy resin is E51 epoxy resin, the epoxy equivalent is 175-210, and the epoxy value is 0.48-0.51.

Particularly preferably, the dioctyl ester is one of dioctyl phthalate, dioctyl adipate or dioctyl azelate.

Specifically, the release agent is methyl silicone oil.

Specifically, the environment-friendly plasticizer is environment-friendly plasticizer TP-95.

Particularly optimized, 2402 phenolic resin is adopted as tackifying resin.