阅读说明：本技术 一种具有特种粘合复合树脂的制备方法 (Preparation method of composite resin with special adhesion ) 是由 宫相勤 徐伟 于 2019-09-06 设计创作，主要内容包括：本发明提供一种具有特种粘合复合树脂的制备方法,步骤如下：(1)取富含萜烯的馏分1000份,碳五馏分500份,液体三氯化铝1份,搅拌反应完毕后加入乙醇2份,恒温搅拌,静置分层,取下层液体减压蒸馏,得粘合树脂；(2)取步骤(1)得到的粘合树脂600份,与苯乙烯-茚树脂150份,炔烃树脂150份,1102树脂100份混合,在温度200~260℃条件下反应得到混合粘合树脂；(3)取步骤(2)得到的粘合树脂800份,与白炭黑200份在温度260-280℃条件下反应得具有特种粘合复合树脂。本发明制备得到的粘合复合树脂具有初粘、终粘结力,胶料挺性优异,可用于橡胶内胎制造、丁基橡胶内胎和高强力丁基内胎制造,简化工序,操作简单,利于提高成品率。(The invention provides a preparation method of special adhesive composite resin, which comprises the following steps of (1) taking 1000 parts of fraction rich in terpene, 500 parts of carbon five fraction and 1 part of liquid aluminum trichloride, adding 2 parts of ethanol after stirring reaction, stirring at constant temperature, standing for layering, and distilling the liquid on the lower layer under reduced pressure to obtain adhesive resin, (2) taking 600 parts of adhesive resin obtained in the step (1), mixing with 150 parts of styrene-indene resin, 150 parts of alkyne resin and 100 parts of 1102 resin, and reacting at the temperature of 200 ~ 260 ℃ to obtain mixed adhesive resin, and (3) taking 800 parts of adhesive resin obtained in the step (2), and reacting with 200 parts of white carbon black at the temperature of 260 ℃ and 280 ℃ to obtain the special adhesive composite resin.)

1. The preparation method of the special adhesive composite resin is characterized by comprising the following steps:

(1) taking 500 ~ 1000 parts of terpene-rich fraction, 500 ~ 1000 parts of carbon five fraction and 1 part of catalyst, stirring and reacting for 2 ~ 10 hours at-20 ~ +10 ℃ and under the pressure of 1.5 ~ 2 MPa, after the reaction is finished, adding 2 parts of ethanol at-10 ~ +10 ℃, stirring for 1 ~ 2 hours at constant temperature, standing and layering for 2 ~ 3 hours, taking the lower-layer liquid, distilling under reduced pressure at 150 ~ 200 ℃ to remove residual fraction, and obtaining 1000 ~ 1200 parts of yellow initial adhesion resin;

(2) mixing 400 ~ 700 parts of the adhesive resin obtained in the step (1) with 100 ~ 200 parts of styrene-indene resin, 100 ~ 200 parts of alkyne resin and 100 ~ 200 parts of 1102 resin, and reacting at 200 ~ 260 ℃ and 1.5 ~ 2 MPa for 4 ~ 6 hours to obtain final adhesive resin;

(3) taking 700 ~ 800 parts of the mixed adhesive resin obtained in the step (2), and reacting with 200 ~ 300 parts of white carbon black for 25 ~ 45 minutes at the temperature of 260 ~ 280 ℃ to obtain stiff resin;

and (3) mixing the products of the steps (1), (2) and (3) to obtain the composite resin.

2. The method for preparing a special adhesive composite resin as claimed in claim 1, wherein the composite resin comprises the following components in parts by weight, namely, an initial adhesion resin 32% ~ 56%, a final adhesion resin 24% ~ 48%, and a stiff resin 16% ~ 24%.

3. The method for preparing a special adhesive composite resin as claimed in claim 2, wherein the composite resin comprises the following components, by weight, 40% of initial adhesion resin, 40% of final adhesion resin and 20% of stiff resin.

4. The method for preparing special adhesive composite resin according to claim 2, wherein the weight of the special rubber adhesive composite resin is 125 parts, the weight of the initial adhesive resin of the product of the step (1) is 40-70 parts, the weight of the final adhesive resin of the product of the step (2) is 30-60 parts, and the weight of the stiff resin of the product of the step (3) is 20-30 parts.

5. The method for preparing special adhesive composite resin according to claim 4, wherein the weight part of special rubber adhesive composite resin is 125, the weight part of initial adhesive resin is 50, the weight part of final adhesive resin is 50, and the weight part of stiff resin is 25.

6. The method for preparing composite resin with special adhesive function as claimed in claim 1 or 2, wherein the softening point of the adhesive resin obtained in step (1) is 60 ~ 65 ℃.

7. The method for preparing the special adhesive composite resin as claimed in claim 6, wherein the composite resin is in the form of powder particles under normal temperature conditions.

8. The method for preparing special adhesive composite resin as claimed in claim 7, wherein in step (1), the terpene-rich fraction comprises 50% terpene and 50% turpentine by weight, and the fraction flow is 60 ~ 180 ℃.

9. The method as claimed in claim 8, wherein the catalyst is liquid aluminum trichloride.

10. The method as claimed in claim 9, wherein the reaction time in step (3) is 30 minutes.

Technical Field

The invention relates to the technical field of composite resin materials, in particular to a preparation method of a special adhesive composite resin.

Background

For many years, the technology of inner tube joints is more critical in the manufacture of rubber inner tubes and butyl inner tubes (hereinafter referred to as inner tubes), wherein the inner tube cutting technology is particularly important, and the cutting is performed by a cutter, and the cut is required to be neat and not deformed. If deformation occurs, the inner tube is easy to deviate and is uneven when being abutted to the seam, and the defects of pressure bearing, tear resistance, air leakage and the like are caused to generate waste tires. Therefore, the tire needs to meet higher technical indexes when being mixed, and the tire has the following special requirements: (1) the initial adhesion is good, and the joint can be automatically bonded during butt joint; (2) the final adhesion is good, and the strength is enough after the joint is bonded; (3) the rubber material joint is required to be stiff, so that the cutter is not deformed, the connector is not deformed during butt joint, and the connector is vulcanized and molded after being free of obstacles. The special requirements are met, the yield of the inner tube is improved, and waste products are not caused. In order to increase the stiffness of a rubber material joint, the traditional method is to freeze the rubber material joint by using liquid nitrogen in a key link of the inner tire joint, so that the stiffness is increased, the joint is prevented from deviating, the process is complex, and the operation is troublesome. If liquid nitrogen freezing is not used, the stiffness requirement cannot be met. If the rubber Mooney viscosity is correspondingly increased from the rubber mixing process to meet the stiffness requirement, the joint strength will be reduced.

Disclosure of Invention

The invention provides a preparation method of special adhesive composite resin, provides a scheme without using liquid nitrogen for manufacturing a high-performance inner tube, and solves the technical problem of complex working procedures caused by the fact that an inner tube joint needs to be frozen by using liquid nitrogen in the prior art.

The invention is realized by the following steps:

(1) taking 500 ~ 1000 parts of terpene-rich fraction, 500 ~ 1000 parts of carbon five fraction, 1500 parts of the sum of the parts of the terpene-rich fraction and the carbon five fraction and 1 part of catalyst, stirring and reacting for 2 ~ 10 hours at-20 ~ +10 ℃ and under the pressure of 1.5 ~ 2 MPa, after the reaction is finished, adding 2 parts of ethanol at-10 ~ +10 ℃, stirring for 1 ~ 2 hours at constant temperature, standing and layering for 2 ~ 3 hours, taking the lower-layer liquid, distilling under reduced pressure at 150 ~ 200 ℃ for 1000 ~ 1200 5 hours to remove residual fractions to obtain 1000 ~ parts of yellow bonding resin, and obtaining 1200 parts of yellow bonding resin;

(2) mixing 400 ~ 700 parts of the bonding resin obtained in the step (1) with 100 ~ 200 parts of styrene-indene resin, 100 ~ 200 parts of alkyne resin and 100 ~ 200 parts of 1102 resin, and reacting at 200 ~ 260 ℃ and 1.5 ~ 2 MPa for 4 ~ 6 hours to obtain mixed bonding resin;

(3) taking 700 ~ 800 parts of the mixed adhesive resin obtained in the step (2) and 200 ~ 300 parts of white carbon black, wherein the total parts by weight of the adhesive resin and the white carbon black is 1000 parts, and reacting for 25 ~ 45 minutes at the temperature of 260 ~ 280 ℃ to obtain the composite resin with special adhesion;

and (3) mixing the products of the steps (1), (2) and (3) to obtain the composite resin.

Styrene-indene resin is supplied by Qingdahai-Haizhi auxiliary agent company Limited, alkyne resin is a perfect product in the prior art, 1102 resin is carbon five carbon nine copolymer resin, is produced in Japan and can be purchased in the market at present.

As a preferred embodiment, the composite resin comprises the following components in parts by weight, namely 32% ~ 56% of initial adhesion resin, 24% ~ 48% of final adhesion resin and 16% ~ 24% of stiff resin.

As a preferred embodiment, the composite resin comprises the following components in parts by weight, namely, 40% of initial adhesion resin, 40% of final adhesion resin and 20% of stiff resin.

In a preferred embodiment, when 125 parts by weight of the special rubber adhesive composite resin is taken, the initial adhesion resin part of the product of the step (1) is 40-70 parts by weight, the final adhesion resin part of the product of the step (2) is 30-60 parts by weight, and the stiff resin part of the product of the step (3) is 20-30 parts by weight.

In a preferred embodiment, when the weight part of the special rubber adhesive composite resin is 125 parts, the weight part of the initial adhesion resin is 50 parts, the weight part of the final adhesion resin is 50 parts, and the weight part of the stiff resin is 25 parts.

As a preferred embodiment, the softening point of the binder resin obtained in step (1) is 60 ~ 65 ℃.

In a preferred embodiment, the special adhesive composite resin is in the form of powder particles under normal temperature conditions.

In a preferred embodiment, in step (1), the terpene-rich fraction comprises 50% terpene and 50% turpentine by weight, and the fraction flow is 60 ~ 180 deg.C.

As a preferred embodiment, the catalyst is liquid aluminum trichloride.

As a preferred embodiment, the reaction time in step (3) is 30 minutes.

The invention has the beneficial effects that: the composite resin prepared by the method has good initial adhesion and final adhesion, and the stiffness of the inner tube is improved. The composite resin has strong initial adhesion, strong adhesive permeability, good adhesion at normal temperature, high final adhesion and proper stiffness, and can improve the level of the operation of the slitting knife and the process of butt joint. The traditional butyl rubber inner tube bonding process adopts a liquid nitrogen freezing method, and the joint strength is 3.3-3.4 MPa. The composite resin provided by the invention is used, and a normal-temperature joint method is adopted, so that the joint strength can reach 5.6-5.8 MPa. Compared with the traditional process, the method can better meet the requirements of high-performance heavy-duty tires and special tires.

In the traditional cutter process, as the rubber material is too soft and has insufficient stiffness and the Mooney viscosity of 35-38, liquid nitrogen is required to be used for cooling before the cutter. When the Mooney viscosity is increased during rubber mixing, the adhesion is insufficient and the joint strength is reduced. The white carbon black modified adhesive resin improves the stiffness of the rubber material, and the Mooney viscosity reaches 43-48. Therefore, liquid nitrogen cooling is not needed, the cutter is smooth, and the yield of the product and the strength of the joint are improved. The method is used for manufacturing rubber inner tubes and butyl rubber inner tubes, and has the advantages of simplified working procedures, simple operation, yield increased from 70% to 99% and joint strength increased by 50-70%.

Drawings

FIG. 1 is a schematic view of the process flow of the composite resin of the present invention applied to an inner tube connector.

Detailed Description

The technical solutions of the present invention will be described clearly and completely with reference to specific embodiments of the present invention, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention. The parts referred to in the present invention are all parts by weight unless otherwise specified.