A heat-curing method for heat-vulcanized rubber sole glue

Abstract

The present invention relates to the technical field of the preparation of heat-cured rubber base glue, particularly to IPC C09, and more specifically to a heat preservation and curing process for heat-cured rubber base glue. The preparation process of the heat-cured rubber base glue of the present invention includes steps of batching, dispersion, grinding, mixing, temperature-controlled stirring, filling, and warehousing. By adding the temperature-controlled stirring process, the present invention shortens the curing time, reduces the warehouse occupancy, shortens the production time of the heat-cured rubber base glue, and thus improves the production efficiency of the base glue.

Description

Technical Field

[0001] The present invention relates to the technical field of the preparation of heat-cured rubber base glue, in particular to IPC C09, and more specifically to a heat-insulating curing process for heat-cured rubber base glue. Background Art

[0002] Metal components can be seen everywhere in life. In order to enhance the performance of metals in some specific scenarios, in addition to changing the properties of the metals themselves, rubber can also be bonded to the metals, so that the metals have properties such as shock absorption, wear resistance, and impact resistance. The main substance for bonding rubber to metal is heat-cured adhesive. When the heat-cured adhesive is double-coated, the adhesive directly applied to the metal surface is heat-cured rubber base glue.

[0003] The existing patent CN201110029305.1 discloses a phenolic-nitrile rubber heat-cured adhesive and its preparation method. The preparation raw materials include a rubber composition, a phenolic resin, a vulcanizing agent, a tackifying resin, a coupling agent, an antioxidant, a pigment filler, and a solvent. The adhesive is obtained by kneading. The performance of the adhesive just after kneading is not stable.

[0004] The production process flow of the heat-cured rubber base glue in the prior art usually includes batching, dispersion, grinding, mixing, filling, warehousing, curing, and shipping. Due to the difference in the compatibility between some raw materials and solvents in the base glue product, after the production is completed, it is in an incomplete stable state and needs to be placed for a period of time. During this period, it needs to be stored in the warehouse for a certain time, which may cause difficulties in the operation of the warehouse. At the same time, the curing time is relatively long, generally more than twenty days, and the production cycle of the entire heat-cured rubber base glue is long. Summary of the Invention

[0005] In order to solve the problems in the prior art, the first aspect of the present invention provides a heat-insulating curing process for heat-cured rubber base glue, including the following steps: batching, dispersion, grinding, mixing, temperature-controlled stirring, filling, and warehousing.

[0006] Preferably, the specific process of the heat-insulating curing process for heat-cured rubber base glue includes the following steps:

[0007] S1: Batching: Weigh rubber, resin, vulcanizing agent, acid absorbent, and filler; mix the rubber with solvent 1 to form a glue solution.

[0008] S2: Dispersion: Emulsify and homogenize the vulcanizing agent, acid absorbent, pigment filler, resin, and solvent 2 for 1-2 hours to obtain an emulsion.

[0009] S3: Grinding: Grind the emulsion for 3-5 hours to obtain a ground liquid.

[0010] S4: Mixing: Mix the grinding fluid with the glue solution, and perform emulsification and homogenization for 1 to 3 hours to obtain a mixed solution;

[0011] S5: Temperature-controlled stirring: Place the mixed solution at 30 - 40 °C, with a stirring speed of 200 - 400 revolutions per minute and a stirring time of 5 - 20 hours;

[0012] S6: Filling; Storage in warehouse.

[0013] In the present invention, by controlling in step S5 to place the mixed solution at 45 °C and with a stirring time of 10 hours, the curing cycle of the heat-cured rubber is shortened, thereby shortening the entire cycle of preparing the heat-cured rubber base glue, improving the efficiency, reducing the warehouse occupancy rate, and lowering the production cost. The inventor of the present invention creatively discovered that there are differences in the compatibility between some raw materials and solvents in the base glue product. After the production is completed, it is in an unstable state and needs to be left for a period of time so that the various materials in the product will gradually diffuse and move towards a stable state. In the present invention, by controlling the stirring temperature and stirring time, the compatibility between the raw materials and solvents is improved, enabling it to reach a stable state faster, shortening the time for the heat-cured rubber base glue to reach 95% R by nearly 3 times. In addition, by controlling the stirring temperature and stirring time, a 100% R vulcanized bonding area can be achieved in 7 days.

[0014] Preferably, in the said S1, the rubber, resin, vulcanizing agent, acid absorbent, and filler, by mass percentage, are 5 - 10% rubber, 10 - 15% resin, 0.5 - 1% vulcanizing agent, 1 - 3% acid absorbent, and 5 - 12% filler.

[0015] Preferably, the said rubber includes chlorinated rubber.

[0016] Preferably, the said chlorinated rubber includes one or more of chlorinated polyethylene rubber, chlorinated polypropylene rubber, and chlorosulfonated polyethylene rubber.

[0017] Preferably, the mass ratio of the said rubber to solvent 1 is (1 - 2):(2 - 3).

[0018] Preferably, the said solvent 1 is xylene.

[0019] Preferably, the said vulcanizing agent includes organic vulcanizing agent or inorganic vulcanizing agent.

[0020] Preferably, the said inorganic vulcanizing agent includes sulfur or hexamethylenetetramine.

[0021] Preferably, the said acid absorbent includes one or more of zinc oxide, magnesium oxide, calcium oxide, and lead oxide; more preferably, the said acid absorbent is zinc oxide.

[0022] Preferably, the filler includes more than three of carbon black, titanium dioxide, fumed silica, kaolin, and asbestos powder.

[0023] Preferably, the mass ratio of the carbon black, titanium dioxide, and fumed silica is (1-2):(3-8):(1-2).

[0024] Preferably, the resin includes one or both of phenolic resin and epoxy phenolic resin.

[0025] Preferably, the solvent 2 includes one or more of toluene, methyl isobutyl ketone, and ethylbenzene; more preferably, it is methyl isobutyl ketone.

[0026] Preferably, the grinding method is wet grinding method.

[0027] Beneficial effects

[0028] 1. In the present invention, by controlling the temperature of the mixed solution at 45°C in step S5, the curing cycle of the heat-cured rubber is shortened, thereby shortening the entire cycle of preparing the heat-cured rubber, improving the efficiency, reducing the warehouse occupancy rate, and lowering the production cost.

[0029] 2. In the present invention, by controlling the stirring time at 10 hours in step S5, the curing time is shortened. When the stirring time is 6 hours, the time required to reach qualified vulcanized bonding performance is longer than that of the heat-cured rubber base compound with a controlled stirring time of 10 hours. When the stirring time is 14 hours, the time required to reach qualified vulcanized bonding performance is also longer than that of the heat-cured rubber base compound with a controlled stirring time of 10 hours. Description of the drawings

[0030] Figure 1 It is a graph showing the change trend of CPS of the heat-cured rubber base compound prepared in Example 1 with the number of days;

[0031] Figure 2 It is a graph showing the change trend of CPS of the heat-cured rubber base compound prepared in Comparative Example 3 with the number of days;

[0032] Figure 3 It is a graph showing the change of CPS of the heat-cured rubber base compound obtained by the preparation process of Example 1 in 0-30 days;

[0033] Figure 4 It is a graph showing the change of CPS of the heat-cured rubber base compound obtained by the preparation process of Comparative Example 1 in 0-30 days;

[0034] Figure 5 It is a graph showing the change of CPS of the heat-cured rubber base compound obtained by the preparation process of Comparative Example 2 in 0-30 days; Specific embodiments

[0035] Example 1

[0036] The first aspect of the present embodiment provides a heat preservation aging process for a heat-vulcanized rubber base, comprising the following steps:

[0037] S1: Ingredients: weigh rubber, resin, vulcanizing agent, acid absorbent, and filler; mix rubber and xylene to form a rubber solution;

[0038] S2: Dispersion: Emulsify and homogenize the vulcanizing agent, acid absorbent, pigment, filler, resin and solvent for 1 hour to obtain an emulsion;

[0039] S3: grinding: grinding the emulsion for 4.5 hours to obtain a grinding liquid;

[0040] S4: Mixing: adding the grinding liquid to the glue liquid, emulsifying and homogenizing and mixing for 1 hour to obtain a mixed liquid;

[0041] S5: Temperature-controlled stirring: the mixed solution is placed at 45°C, the stirring speed is 200-400 rpm, and the stirring time is 10 hours;

[0042] S6: Filling; warehousing.

[0043] The rubber, resin, vulcanizing agent, acid absorber and filler in S1 are 10% rubber, 10% resin, 1% vulcanizing agent, 3% acid absorber and 6% filler in terms of mass percentage.

[0044] The vulcanizing agent is hexamethylenetetramine.

[0045] The acid scavenger is zinc oxide.

[0046] The filler is carbon black, titanium dioxide and fumed silica.

[0047] The mass ratio of the carbon black, titanium dioxide and fumed silica is 1:3:2.

[0048] The resin is a phenolic resin.

[0049] The solvent is methyl isobutyl ketone.

[0050] The methyl isobutyl ketone is 60% methyl isobutyl ketone by mass percentage.

[0051] The xylene is 10% by mass.

[0052] The rubber is chlorosulfonated polyethylene rubber.

[0053] The grinding method is wet grinding.

[0054] The CAS number of the hexamethylenetetramine is 100-79-0. The CAS number of the carbon black is 1333-86-4. The CAS number of the titanium dioxide is 13463-67-7. The CAS number of the fumed silica is 7631-86-9. The CAS number of the methyl isobutyl ketone is 108-10-1. The phenolic resin is purchased from Shandong Changyao New Materials Co., Ltd., and the model is CY-D2. The chlorosulfonated polyethylene rubber is purchased from Hubei Xinghengye Technology Co., Ltd. The CAS number of the xylene is 1330-20-7.

[0055] Example 2

[0056] The specific implementation method of Example 2 is the same as that of Example 1, except that the stirring time is 6 hours.

[0057] Example 3

[0058] The specific implementation method of Example 3 is the same as that of Example 1, except that the stirring time is 14 hours.

[0059] Comparative Example 1

[0060] The specific implementation method of Comparative Example 1 is the same as that of Example 1, except that the mixed solution is stirred at 5°C for 10 hours.

[0061] Comparative Example 2

[0062] The specific implementation method of Comparative Example 2 is the same as that of Example 1, except that the mixed solution is stirred at 25°C for 10 hours.

[0063] Comparative Example 3

[0064] The specific implementation method of Comparative Example 3 is the same as that of Example 1, except that in the heat-curing process of the heat-cured rubber base compound, the process is batching, dispersion, grinding, stirring and mixing, filling, warehousing, curing, and shipping.

[0065] The curing process is to place the heat-cured rubber base compound at 25°C for 20 days.

[0066] Performance Test

[0067] 1. Rotational Viscosity (CPS) Test

[0068] According to the national standard GB / T-2794-2013, measure the rotational viscosity (CPS) of the heat-cured rubber base compound prepared in Example 1 and Comparative Example 3, and conduct 5 parallel tests and 3 parallel tests respectively. Each group of parallel experiments is represented by a line of different colors. The results are shown in Figure 1 、 Figure 2 。From Figure 1 、 Figure 2It can be seen that the CPS stable period in Example 1 decreased from 20 days to 7 days.

[0069] 2. Vulcanization bonding performance test

[0070] Bonding material: NBR - nitrile rubber

[0071] Measure the initial adhesion data of the heat - vulcanized rubber base rubber prepared in Example 1 and Comparative Example 3 after curing for 1 - 7 days.

[0072] Test method: Before testing, use a stirring knife to stir thoroughly for 2 minutes until the product is completely uniform. Select the substrate (zinc sheet) for brushing operation according to the bonding vulcanization requirements of each product. Ensure complete drying during brushing, and the coating thickness is 10μm. Turn on the vulcanizer, set it to 160°C for 10 minutes. After the vulcanizing agent reaches the temperature, neatly place the processed rubber horizontally into the mold (with the rubber grinding surface facing up). Place the brushed surface of the substrate in contact with the grinding surface of the rubber. At this time, wear heat - insulating gloves and place the mold on the vulcanizer platform. The iron sheet is below and the rubber is above. Push the pressure rod to the pressure - increasing position and press the vulcanizer operation button. The platform rises to increase the pressure. After the vulcanization time ends, press the stop button, and push the pressure rod to the pressure - decreasing position. Wait for 5 seconds, and the vulcanization platform resets. Wear heat - insulating gloves and take out the mold and place it on the workbench to cool. After vulcanization, wait for the product to cool completely and then conduct peeling. After peeling, use a reading ruler to take readings for the substrate.

[0073] Record the results of Example 1 in Table 1 and the results of Comparative Example 3 in Table 2. The vulcanization bonding of the heat - vulcanized rubber base rubber in Example 1 meets the requirements of the 7 - day curing cycle, and the bonding performance requirements are met after 3 days with a stirring time of 10 hours.

[0074] 3. Measure the CPS values of the heat - vulcanized rubber base rubber obtained from the preparation processes of Example 1 and Comparative Examples 1 and 2 from 0 to 30 days, and then conduct 6 parallel experiments. The results are shown in Figure 3 、 Figure 4 、 Figure 5 。

[0075] Table 1

[0076]

[0077] Table 2

[0078]

Claims

1. A heat-curing method process for hot-vulcanized rubber base glue, characterized in that, it includes the following steps: batching, dispersing, grinding, mixing, temperature-controlled stirring, filling, and warehousing; The specific process of the heat-curing method process for hot-vulcanized rubber base glue, includes the following steps: S1: Batching: Weigh rubber, resin, vulcanizing agent, acid absorbent, and filler; Mix the rubber with solvent 1 to form a glue solution; S2: Dispersing: Emulsify and homogenize the vulcanizing agent, acid absorbent, filler, resin, and solvent 2 for 1-2 hours to obtain an emulsion; S3: Grinding: Grind the emulsion for 3-5 hours to obtain a ground liquid; S4: Mixing: Mix the ground liquid with the glue solution and emulsify and homogenize for 1-3 hours to obtain a mixed liquid; S5: Temperature-controlled stirring: Place the mixed liquid at 45°C, with a stirring speed of 200-400 rpm and a stirring time of 10 hours; S6: Filling and warehousing; In the above S1, the rubber, resin, vulcanizing agent, acid absorbent, and filler, by mass percentage, are 5-10% rubber, 10-15% resin, 0.5-1% vulcanizing agent, 1-3% acid absorbent, and 5-12% filler; The above vulcanizing agent includes sulfur or hexamine; The above acid absorbent includes one or more of zinc oxide, magnesium oxide, calcium oxide, and lead oxide; The above filler is carbon black, titanium dioxide, and fumed silica; The mass ratio of carbon black, titanium dioxide, and fumed silica is (1-2):(3-8):(1-2); The above resin includes one or two of phenolic resin and epoxy phenolic resin; The above rubber includes chlorinated rubber; The chlorinated rubber includes one or more of chlorinated polyethylene rubber, chlorinated polypropylene rubber, and chlorosulfonated polyethylene rubber.

2. The heat-curing method process for hot-vulcanized rubber base glue according to claim 1, characterized in that, The above solvent includes one or more of toluene, methyl isobutyl ketone, and ethylbenzene.

3. The heat-curing method process for hot-vulcanized rubber base glue according to claim 1, characterized in that, The mass ratio of the above rubber to solvent 1 is (1-2):(2-3).

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