CN110760268A - Preparation method of heat-resistant rubber binder - Google Patents
Preparation method of heat-resistant rubber binder Download PDFInfo
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- CN110760268A CN110760268A CN201911063208.7A CN201911063208A CN110760268A CN 110760268 A CN110760268 A CN 110760268A CN 201911063208 A CN201911063208 A CN 201911063208A CN 110760268 A CN110760268 A CN 110760268A
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J4/00—Adhesives based on organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond ; adhesives, based on monomers of macromolecular compounds of groups C09J183/00 - C09J183/16
- C09J4/06—Organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond in combination with a macromolecular compound other than an unsaturated polymer of groups C09J159/00 - C09J187/00
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
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Abstract
The invention discloses a preparation method of a heat-resistant rubber binder, belonging to the technical field of binder preparation. The invention adds silicon dioxide powder, reacts in alkali liquor at high temperature and high pressure, makes silicate ions generate silicic acid by adjusting pH value, protects part of components in the rubber binder by silicon dioxide, and improves the heat resistance of the rubber binder by the good thermal stability and chemical stability of the silicon dioxide.
Description
Technical Field
The invention discloses a preparation method of a heat-resistant rubber binder, belonging to the technical field of binder preparation.
Background
The rubber adhesive is widely applied in the preparation process of rubber products, and the chloroprene rubber adhesive is used as one of the rubber adhesives and is commonly used in the rubber adhesives, but the chloroprene rubber adhesive used in the prior art is usually formed by singly combining chloroprene rubber and a solvent, so that the phenomena of infirm bonding, easy loosening and the like are often caused in the process of bonding the rubber products, particularly in the process of bonding different rubber products, the bonding effect is poor, and the product quality is greatly influenced.
The neoprene adhesive is a kind of rubber adhesive with large dosage, which has the characteristics of strong initial adhesion, high bonding strength, weather resistance and the like, and can not be replaced by other adhesives, thus having wide application. The traditional preparation method of the chloroprene rubber adhesive is to use a rubber mixing mill to plasticate and mix rubber sheets for shearing molecular chains, so as to destroy gel in a polymer and reduce the viscosity of a solution. The accelerator is added during the mixing process, and then the rubber compound sheet is cut into strips and dissolved in the solvent in a closed container with a stirrer. The method has the advantages of high manufacturing cost and equipment investment, high energy consumption, complex process and low efficiency. With the development of economy, the consumption of the chloroprene rubber adhesive is more and more, while the traditional chloroprene rubber adhesive mostly uses single chloroprene rubber, and the solvent mostly uses benzene, so that certain pollution is caused to the environment, certain differences exist between the quality and the performance of the chloroprene rubber adhesive and the foreign like products, the chloroprene rubber adhesive cannot meet the requirements in the actual use process, and the use is limited to a certain extent.
There is also a class of adhesives, and the concept of using essentially no benzene as a solvent has been proposed, for example application No. cn200410039520.x provides a new formulation and preparation method for neoprene adhesives. The components and the weight percentage content are as follows: 2442 chloroprene rubber 16.5-18.5%, cyclopentane B type solvent 46-52%, methyl ethyl ketone 2-4%, ethyl acetate 16-18%, 120# gasoline 3-5%, 2402 tert-butyl phenolic resin 7.5-9.5%, magnesium oxide 1.5-5.5%, zinc oxide 0.2-0.5%, benzoic acid 0.03-0.05%, and water 0.01-0.03%. The technical scheme uses ten raw materials, and in the aspect of performance, the low-temperature resistance performance index can not meet the use requirement, and the bonding performance of the adhesive is poor when the adhesive is used in a humid environment, so that the use range and the environment are limited to a certain extent.
The treatise on the principle and process for producing chloroprene rubber type rubber adhesives describes the material series of polymer materials and engineering specialties. It is also proposed that benzene is not used as a solvent, and in the document, the optimal formula (parts by mass) of the chloroprene rubber adhesive for woodworking is obtained as follows: the neoprene 100, the terpene-phenolic resin 40, the light calcium carbonate 20 and the mixed solvent 550 which is composed of ethyl acetate and 120 solvent oil according to the mass ratio of 67: 33, and all performance indexes of the neoprene 550 can meet the requirements of the industry standard LY/T1206-2008 'neoprene adhesive for carpentry'. The method also needs heating, and the preparation time of dissolution needs about 20 hours.
In addition, most of high-grade adhesives use imported chloroprene rubber, so that the cost is high, the viscosity retention time is short, and the high-grade adhesives cannot resist high temperature.
Therefore, the invention of the rubber adhesive which is firm in bonding, not easy to loosen and good in high-temperature resistance is necessary for the technical field of adhesive preparation.
Disclosure of Invention
The technical problems to be solved by the invention are as follows: aiming at the defects that the bonding effect of the rubber adhesive is poor and the high temperature resistance of the rubber adhesive is poor due to the fact that the existing rubber adhesive is not firm in bonding and easy to loosen, and the preparation method of the heat-resistant rubber adhesive is provided.
In order to solve the technical problems, the invention adopts the technical scheme that:
the preparation method of the heat-resistant rubber binder comprises the following steps:
putting the self-made bonding product, polyisocyanate adhesive and chloroprene rubber into a mixing roll, mixing for 50-60 min at the temperature of 110-120 ℃ to obtain a prefabricated product, putting the prefabricated product, zinc oxide, methyl methacrylate and acetone into a reaction kettle, raising the temperature in the reaction kettle to 130-150 ℃, stirring for 2-3 h at the rotating speed of 400-500 r/min by using a stirring device, and discharging to obtain the heat-resistant rubber binder;
the preparation method of the self-made bonding product comprises the following specific steps:
(1) putting a hot reactant and silicon dioxide powder into a reaction kettle, filling nitrogen into the reaction kettle to increase the air pressure in the reaction kettle to 1.0-1.2 MPa, increasing the temperature in the reaction kettle to 150-170 ℃, carrying out constant-temperature and constant-pressure reaction for 80-100 min to obtain reaction slurry, dropwise adding hydrochloric acid with the mass fraction of 10-15% into the reaction kettle to adjust the pH value to 3-4, and stirring for 30-40 min at the rotating speed of 500-600 r/min by using a stirring device to obtain a prefabricated mixed solution;
(2) putting the prefabricated mixed liquid and aluminum chloride into a beaker, putting the beaker into an ultrasonic oscillator, oscillating and mixing for 6-8 h under the condition that the frequency is 36-40 kHz, dropwise adding hydrochloric acid with the mass fraction of 6-10% into the beaker to adjust the pH value to 2-3 to prepare a reaction liquid to be subjected to enzymolysis, putting the reaction liquid to be subjected to enzymolysis and pepsin into an enzymolysis tank according to the mass ratio of 15:1, putting the enzymolysis tank into a greenhouse with the indoor temperature of 35-40 ℃, and standing at constant temperature for 12-14 h to prepare an enzymolysis liquid;
(3) putting the enzymatic hydrolysate into a beaker, putting the beaker into a resistance heating sleeve, raising the temperature in the heating sleeve to 95-100 ℃, simultaneously stirring for 40-50 min at the rotating speed of 300-400 r/min by using a stirrer, dropwise adding a sodium hydroxide solution with the mass fraction of 5-10% into the beaker after stirring to adjust the pH value to 6.5-7.0, putting the beaker into a vacuum drying oven, and concentrating and drying for 12-14 h under the conditions of the temperature of 80-100 ℃ and the vacuum degree of 100-150 Pa to prepare a self-made bonding product;
the specific preparation steps of the thermal reactant are as follows:
(1) putting soybean flour and soybean straws into an oven, drying for 10-12 h at the temperature of 60-70 ℃, putting into a crusher after drying, crushing and mixing to obtain a mixed material, putting the mixed material and deionized water into a beaker according to the mass ratio of 1:5, and stirring for 50-60 min at the rotating speed of 1100-1200 r/min by using a stirring device to obtain mixed slurry;
(2) putting the beaker into a water bath kettle with the water bath temperature of 95-100 ℃, standing for 2-3 hours at constant temperature to prepare reaction slurry, dropwise adding a sodium hydroxide solution with the mass fraction of 10-16% into the reaction kettle to adjust the pH value, sealing the reaction kettle, raising the temperature in the reaction kettle to 160-180 ℃, and reacting at high temperature for 100-120 min to prepare a thermal reactant.
Preferably, the self-made bonding product is 8-10 parts by weight, the polyisocyanate adhesive is 30-35 parts by weight, and the chloroprene rubber is 20-24 parts by weight.
Preferably, the weight parts of the prefabricated product are 40-42 parts, 2-4 parts of zinc oxide, 8-10 parts of methyl methacrylate and 3-5 parts of acetone.
The mass ratio of the hot reactant to the silicon dioxide powder in the specific preparation step (1) of the self-made bonding product is 15: 1.
The mass ratio of the prefabricated mixed liquid to the aluminum chloride in the specific preparation step (2) of the self-made bonding product is 30: 1.
The reaction liquid to be subjected to enzymolysis and the pepsin in the specific preparation step (2) of the self-made bonding product are 15:1 in mass ratio.
The mass ratio of the soybean flour to the soybean straw in the specific preparation step (1) of the hot reactant is 1: 10.
The mass ratio of the mixed material to the deionized water in the specific preparation step (1) of the thermal reactant is 1: 5.
The pH value of the dropwise added sodium hydroxide solution with the mass fraction of 10-16% is further preferably adjusted to be 12-13 in the specific preparation step (2) of the thermal reactant.
The beneficial technical effects of the invention are as follows:
(1) the invention firstly dries and crushes soybean meal and soybean straw, mixes and stirs the soybean meal and soybean straw to prepare mixed serous fluid, then heats the mixed serous fluid at high temperature, adds alkali liquor to prepare hot reactant, then mixes the hot reactant and silicon dioxide to process at high temperature and high pressure, adjusts pH value after processing to prepare prefabricated mixed fluid, then mixes the prefabricated mixed fluid and aluminum chloride, adds pepsin to prepare enzymolysis fluid, then heats the enzymolysis fluid at high temperature to adjust pH value to neutrality, concentrates and dries to prepare self-made bonding product, finally mixes the self-made bonding product, polyisocyanate adhesive and other materials to prepare prefabricated product, finally mixes and stirs the prefabricated product, zinc oxide and other auxiliary agents at high temperature to prepare the heat-resistant rubber binder The vegetable fiber is separated, the soybean protein is subjected to enzymolysis by utilizing pepsin to generate components such as amino acid and polypeptide, the number of carboxyl and amino functional groups in an organic matter is increased, chemical bonding forces such as hydrogen bonds, covalent bonds and intermolecular forces are formed between the functional groups such as the carboxyl and the amino and the components in the rubber adhesive to increase the bonding strength among the components in the rubber adhesive, the phenomena of insecurity and degumming of the adhesive in the use process are avoided, meanwhile, the components such as the vegetable fiber are continuously decomposed under the high-temperature condition to generate organic compounds with shorter carbon chains, meanwhile, a large number of functional groups such as the carboxyl and the hydroxyl are grafted on a peptide chain, the number of the functional groups is further increased, the bonding strength among the components is improved, and the firmness of the rubber adhesive is increased;
(2) the invention adds silicon dioxide powder, reacts at high temperature and high pressure in alkali liquor, further decomposes plant fiber and polypeptide components, simultaneously adsorbs silicate ions to bond in fiber molecules and polypeptide components through electrostatic ions, then adjusts the pH value to enable the silicate ions to generate silicic acid, the silicic acid is decomposed to generate silicon dioxide and water, nano silicon dioxide particles are bonded in organic components, silicon dioxide particles are filled among the fiber components, the polypeptide and other components, partial components in the rubber binder are protected by the silicon dioxide, the heat resistance of the rubber binder is improved through the good thermal stability and chemical stability of the silicon dioxide, and the invention has wide application prospect.
Detailed Description
Putting soybean flour and soybean straws into an oven according to the mass ratio of 1:10, drying for 10-12 h at the temperature of 60-70 ℃, putting the dried soybean flour and soybean straws into a crusher, crushing and mixing to obtain a mixed material, putting the mixed material and deionized water into a beaker according to the mass ratio of 1:5, and stirring for 50-60 min at the rotating speed of 1100-1200 r/min by using a stirring device to obtain mixed slurry; putting the beaker into a water bath kettle with a water bath temperature of 95-100 ℃, standing for 2-3 h at a constant temperature to prepare reaction slurry, dropwise adding a sodium hydroxide solution with the mass fraction of 10-16% into the reaction kettle to adjust the pH value to 12-13, sealing the reaction kettle, raising the temperature in the reaction kettle to 160-180 ℃, and reacting at a high temperature for 100-120 min to prepare a thermal reactant; putting the thermal reactant and silicon dioxide powder into a reaction kettle according to a mass ratio of 15:1, filling nitrogen into the reaction kettle to increase the air pressure in the reaction kettle to 1.0-1.2 MPa, increasing the temperature in the reaction kettle to 150-170 ℃, carrying out constant-temperature and constant-pressure reaction for 80-100 min to obtain reaction slurry, dropwise adding hydrochloric acid with the mass fraction of 10-15% into the reaction kettle to adjust the pH value to 3-4, and stirring with a stirring device at the rotating speed of 500-600 r/min for 30-40 min to obtain a prefabricated mixed solution; putting the prefabricated mixed liquid and aluminum chloride into a beaker according to the mass ratio of 30:1, putting the beaker into an ultrasonic oscillator, oscillating and mixing for 6-8 h under the condition that the frequency is 36-40 kHz, dropwise adding hydrochloric acid with the mass fraction of 6-10% into the beaker to adjust the pH value to 2-3 to prepare a reaction liquid to be subjected to enzymolysis, putting the reaction liquid to be subjected to enzymolysis and pepsin into an enzymolysis tank according to the mass ratio of 15:1, putting the enzymolysis tank into a greenhouse with the indoor temperature of 35-40 ℃, and standing for 12-14 h at constant temperature to prepare an enzymolysis liquid; placing the enzymatic hydrolysate in a beaker, placing the beaker in a resistance heating sleeve, raising the temperature in the heating sleeve to 95-100 ℃, simultaneously stirring for 40-50 min at the rotating speed of 300-400 r/min by using a stirrer, dropwise adding a sodium hydroxide solution with the mass fraction of 5-10% into the beaker after stirring to adjust the pH value to 6.5-7.0, placing the beaker in a vacuum drying oven, and concentrating and drying for 12-14 h under the conditions of the temperature of 80-100 ℃ and the vacuum degree of 100-150 Pa to obtain a self-made bonding product; putting 8-10 parts by weight of the self-made bonding product, 30-35 parts by weight of polyisocyanate adhesive and 20-24 parts by weight of chloroprene rubber into a mixing roll, mixing for 50-60 min at the temperature of 110-120 ℃ to obtain a prefabricated product, putting 40-42 parts by weight of the prefabricated product, 2-4 parts by weight of zinc oxide, 8-10 parts by weight of methyl methacrylate and 3-5 parts by weight of acetone into a reaction kettle, raising the temperature in the reaction kettle to 130-150 ℃, stirring for 2-3 h at the rotating speed of 400-500 r/min by using a stirring device, and discharging to obtain the heat-resistant rubber binder.
Example 1
Preparation of the thermal reactants:
putting soybean flour and soybean straw into an oven according to the mass ratio of 1:10, drying for 10h at the temperature of 60 ℃, putting into a pulverizer after drying, pulverizing and mixing to obtain a mixed material, putting the mixed material and deionized water into a beaker according to the mass ratio of 1:5, and stirring for 50min at the rotating speed of 1100r/min by using a stirring device to obtain mixed slurry;
putting the beaker into a water bath kettle with the water bath temperature of 95 ℃, standing at constant temperature for 2 hours to prepare reaction slurry, dropwise adding a sodium hydroxide solution with the mass fraction of 10% into a reaction kettle to adjust the pH value to 12, sealing the reaction kettle, raising the temperature in the reaction kettle to 160 ℃, and reacting at high temperature for 100min to prepare a thermal reactant;
preparation of a self-made binding product:
putting the thermal reactant and silicon dioxide powder into a reaction kettle according to the mass ratio of 15:1, filling nitrogen into the reaction kettle to increase the air pressure in the reaction kettle to 1.0MPa, increasing the temperature in the reaction kettle to 150 ℃, carrying out constant-temperature and constant-pressure reaction for 80min to obtain reaction slurry, dropwise adding hydrochloric acid with the mass fraction of 10% into the reaction kettle to adjust the pH value to 3, and stirring for 30min at the rotating speed of 500r/min by using a stirring device to obtain a prefabricated mixed solution;
putting the prefabricated mixed liquid and aluminum chloride into a beaker according to the mass ratio of 30:1, putting the beaker into an ultrasonic oscillator, oscillating and mixing for 6 hours under the condition that the frequency is 36kHz, dropwise adding hydrochloric acid with the mass fraction of 6% into the beaker to adjust the pH value to 2 to prepare a reaction liquid to be subjected to enzymolysis, putting the reaction liquid to be subjected to enzymolysis and pepsin into an enzymolysis tank according to the mass ratio of 15:1, putting the enzymolysis tank into a greenhouse with the indoor temperature of 35 ℃, and standing at constant temperature for 12 hours to prepare an enzymolysis liquid;
placing the enzymatic hydrolysate in a beaker, placing the beaker in a resistance heating sleeve, raising the temperature in the heating sleeve to 95 ℃, simultaneously stirring for 40min at the rotating speed of 300r/min by using a stirrer, dropwise adding a sodium hydroxide solution with the mass fraction of 5% into the beaker after stirring to adjust the pH value to 6.5, placing the beaker in a vacuum drying oven, and concentrating and drying for 12h under the conditions of the temperature of 80 ℃ and the vacuum degree of 100Pa to obtain a self-made binding product;
preparation of heat-resistant rubber binder:
putting 8 parts by weight of the self-made bonding product, 30 parts by weight of polyisocyanate and 20 parts by weight of chloroprene rubber into a mixing roll, mixing for 50min at the temperature of 110 ℃ to obtain a prefabricated product, putting 40 parts by weight of the prefabricated product, 2 parts by weight of zinc oxide, 8 parts by weight of methyl methacrylate and 3 parts by weight of acetone into a reaction kettle, raising the temperature in the reaction kettle to 130 ℃, stirring for 2h at the rotating speed of 400r/min by using a stirring device, and discharging to obtain the heat-resistant rubber binder.
Example 2
Preparation of the thermal reactants:
putting soybean flour and soybean straws into an oven according to the mass ratio of 1:10, drying for 11 hours at the temperature of 65 ℃, putting into a crusher after drying, crushing and mixing to obtain a mixed material, putting the mixed material and deionized water into a beaker according to the mass ratio of 1:5, and stirring for 55 minutes by a stirring device at the rotating speed of 1150r/min to obtain mixed slurry;
putting the beaker into a water bath kettle with the water bath temperature of 97 ℃, standing at constant temperature for 2.5h to prepare reaction slurry, dropwise adding 13% by mass of sodium hydroxide solution into a reaction kettle to adjust the pH value to 12, sealing the reaction kettle, raising the temperature in the reaction kettle to 170 ℃, and reacting at high temperature for 110min to prepare a thermal reactant;
preparation of a self-made binding product:
putting the thermal reactant and silicon dioxide powder into a reaction kettle according to the mass ratio of 15:1, filling nitrogen into the reaction kettle to increase the air pressure in the reaction kettle to 1.1MPa, increasing the temperature in the reaction kettle to 160 ℃, carrying out constant-temperature and constant-pressure reaction for 90min to obtain reaction slurry, dropwise adding hydrochloric acid with the mass fraction of 12% into the reaction kettle to adjust the pH value to 3, and stirring for 35min at the rotating speed of 550r/min by using a stirring device to obtain a prefabricated mixed solution;
putting the prefabricated mixed liquid and aluminum chloride into a beaker according to the mass ratio of 30:1, putting the beaker into an ultrasonic oscillator, oscillating and mixing for 7 hours under the condition of the frequency of 38kHz, dropwise adding hydrochloric acid with the mass fraction of 8% into the beaker to adjust the pH value to 2 to prepare a reaction liquid to be subjected to enzymolysis, putting the reaction liquid to be subjected to enzymolysis and pepsin into an enzymolysis tank according to the mass ratio of 15:1, putting the enzymolysis tank into a greenhouse with the indoor temperature of 37 ℃, and standing at constant temperature for 13 hours to prepare an enzymolysis liquid;
placing the enzymatic hydrolysate in a beaker, placing the beaker in a resistance heating sleeve, raising the temperature in the heating sleeve to 97 ℃, simultaneously stirring for 45min at the rotating speed of 350r/min by using a stirrer, dropwise adding a sodium hydroxide solution with the mass fraction of 7% into the beaker after stirring to adjust the pH value to 6.7, placing the beaker in a vacuum drying box, and concentrating and drying for 13h under the conditions of the temperature of 90 ℃ and the vacuum degree of 120Pa to obtain a self-made binding product;
preparation of heat-resistant rubber binder:
and (2) putting 9 parts of the self-made bonding product, 32 parts of polyisocyanate and 22 parts of chloroprene rubber into a mixing roll, mixing for 55min at the temperature of 115 ℃ to obtain a prefabricated product, putting 41 parts of the prefabricated product, 3 parts of zinc oxide, 9 parts of methyl methacrylate and 4 parts of acetone into a reaction kettle, raising the temperature in the reaction kettle to 140 ℃, stirring for 2.5h at the rotating speed of 450r/min by using a stirring device, and discharging to obtain the heat-resistant rubber bonding agent.
Example 3
Preparation of the thermal reactants:
putting soybean flour and soybean straws into an oven according to the mass ratio of 1:10, drying for 12h at the temperature of 70 ℃, putting into a pulverizer after drying, pulverizing and mixing to obtain a mixed material, putting the mixed material and deionized water into a beaker according to the mass ratio of 1:5, and stirring for 60min at the rotating speed of 1200r/min by using a stirring device to obtain mixed slurry;
putting the beaker into a water bath kettle with the water bath temperature of 100 ℃, standing for 3 hours at constant temperature to prepare reaction slurry, dropwise adding a sodium hydroxide solution with the mass fraction of 16% into a reaction kettle to adjust the pH value to 13, sealing the reaction kettle, raising the temperature in the reaction kettle to 180 ℃, and reacting at high temperature for 120min to prepare a thermal reactant;
preparation of a self-made binding product:
putting the thermal reactant and silicon dioxide powder into a reaction kettle according to the mass ratio of 15:1, filling nitrogen into the reaction kettle to increase the air pressure in the reaction kettle to 1.2MPa, increasing the temperature in the reaction kettle to 170 ℃, carrying out constant-temperature and constant-pressure reaction for 100min to obtain reaction slurry, dropwise adding hydrochloric acid with the mass fraction of 15% into the reaction kettle to adjust the pH value to 4, and stirring for 40min at the rotating speed of 600r/min by using a stirring device to obtain a prefabricated mixed solution;
putting the prefabricated mixed liquid and aluminum chloride into a beaker according to the mass ratio of 30:1, putting the beaker into an ultrasonic oscillator, oscillating and mixing for 8 hours under the condition of 40kHz frequency, dropwise adding hydrochloric acid with the mass fraction of 10% into the beaker to adjust the pH value to 3 to prepare a reaction liquid to be subjected to enzymolysis, putting the reaction liquid to be subjected to enzymolysis and pepsin into an enzymolysis tank according to the mass ratio of 15:1, putting the enzymolysis tank into a greenhouse with the indoor temperature of 40 ℃, and standing for 14 hours at constant temperature to prepare an enzymolysis liquid;
placing the enzymatic hydrolysate in a beaker, placing the beaker in a resistance heating sleeve, raising the temperature in the heating sleeve to 100 ℃, simultaneously stirring for 50min at the rotating speed of 400r/min by using a stirrer, dropwise adding a sodium hydroxide solution with the mass fraction of 10% into the beaker after stirring to adjust the pH value to 7.0, placing the beaker in a vacuum drying oven, and concentrating and drying for 14h under the conditions of the temperature of 100 ℃ and the vacuum degree of 150Pa to obtain a self-made binding product;
preparation of heat-resistant rubber binder:
putting 10 parts by weight of the self-made bonding product, 35 parts by weight of polyisocyanate and 24 parts by weight of chloroprene rubber into a mixing roll, mixing for 60min at the temperature of 120 ℃ to obtain a prefabricated product, putting 42 parts by weight of the prefabricated product, 4 parts by weight of zinc oxide, 10 parts by weight of methyl methacrylate and 5 parts by weight of acetone into a reaction kettle, raising the temperature in the reaction kettle to 150 ℃, stirring for 3h at the rotating speed of 500r/min by using a stirring device, and discharging to obtain the heat-resistant rubber binder.
Comparative example 1: essentially the same procedure as in example 2, except for the absence of the hot reactant.
Comparative example 2: essentially the same procedure as in example 2, except that the home-made cementitious product was absent.
Comparative example 3: a heat-resistant rubber adhesive produced by Shandong company.
And (3) testing the bonding property: the rubber adhesives prepared in examples and comparative examples were coated on test pieces, respectively, and after covering, they were dried with hot air at 45 c, and the test pieces were placed on a rubber tensile machine to measure peel strength, and the results are shown in table 1.
And (3) high temperature resistance test: the rubber adhesives prepared in examples and comparative examples were coated on test pieces, respectively, covered, dried with hot air at 45 ℃, placed in an oven, and tested for peel strength.
Table 1: results of measuring the Properties of rubber Binders
| Detecting items | Example 1 | Example 2 | Example 3 | Comparative example 1 | Comparative example 2 | Comparative example 3 |
| Peel strength (kN/m) | 3.49 | 3.52 | 3.56 | 1.78 | 1.53 | 1.89 |
| High temperature peel strength (kN/m) | 3.05 | 3.08 | 3.12 | 0.98 | 1.32 | 1.54 |
In summary, it can be seen from table 1 that the rubber binder of the present invention has the advantages of firm adhesion, low possibility of loosening, good adhesion effect, high peel strength, good high temperature resistance, high peel strength after high temperature baking, and wide application prospects.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, but rather as the subject matter of the invention is to be construed in all aspects and as broadly as possible, and all changes, equivalents and modifications that fall within the true spirit and scope of the invention are therefore intended to be embraced therein.
Claims (9)
1. A preparation method of a heat-resistant rubber binder is characterized by comprising the following specific preparation steps:
putting the self-made bonding product, polyisocyanate adhesive and chloroprene rubber into a mixing roll, mixing for 50-60 min at the temperature of 110-120 ℃ to obtain a prefabricated product, putting the prefabricated product, zinc oxide, methyl methacrylate and acetone into a reaction kettle, raising the temperature in the reaction kettle to 130-150 ℃, stirring for 2-3 h at the rotating speed of 400-500 r/min by using a stirring device, and discharging to obtain the heat-resistant rubber binder;
the preparation method of the self-made bonding product comprises the following specific steps:
(1) putting a hot reactant and silicon dioxide powder into a reaction kettle, filling nitrogen into the reaction kettle to increase the air pressure in the reaction kettle to 1.0-1.2 MPa, increasing the temperature in the reaction kettle to 150-170 ℃, carrying out constant-temperature and constant-pressure reaction for 80-100 min to obtain reaction slurry, dropwise adding hydrochloric acid with the mass fraction of 10-15% into the reaction kettle to adjust the pH value to 3-4, and stirring for 30-40 min at the rotating speed of 500-600 r/min by using a stirring device to obtain a prefabricated mixed solution;
(2) putting the prefabricated mixed liquid and aluminum chloride into a beaker, putting the beaker into an ultrasonic oscillator, oscillating and mixing for 6-8 h under the condition that the frequency is 36-40 kHz, dropwise adding hydrochloric acid with the mass fraction of 6-10% into the beaker to adjust the pH value to 2-3 to prepare a reaction liquid to be subjected to enzymolysis, putting the reaction liquid to be subjected to enzymolysis and pepsin into an enzymolysis tank according to the mass ratio of 15:1, putting the enzymolysis tank into a greenhouse with the indoor temperature of 35-40 ℃, and standing at constant temperature for 12-14 h to prepare an enzymolysis liquid;
(3) putting the enzymatic hydrolysate into a beaker, putting the beaker into a resistance heating sleeve, raising the temperature in the heating sleeve to 95-100 ℃, simultaneously stirring for 40-50 min at the rotating speed of 300-400 r/min by using a stirrer, dropwise adding a sodium hydroxide solution with the mass fraction of 5-10% into the beaker after stirring to adjust the pH value to 6.5-7.0, putting the beaker into a vacuum drying oven, and concentrating and drying for 12-14 h under the conditions of the temperature of 80-100 ℃ and the vacuum degree of 100-150 Pa to prepare a self-made bonding product;
the specific preparation steps of the thermal reactant are as follows:
(1) putting soybean flour and soybean straws into an oven, drying for 10-12 h at the temperature of 60-70 ℃, putting into a crusher after drying, crushing and mixing to obtain a mixed material, putting the mixed material and deionized water into a beaker according to the mass ratio of 1:5, and stirring for 50-60 min at the rotating speed of 1100-1200 r/min by using a stirring device to obtain mixed slurry;
(2) putting the beaker into a water bath kettle with the water bath temperature of 95-100 ℃, standing for 2-3 hours at constant temperature to prepare reaction slurry, dropwise adding a sodium hydroxide solution with the mass fraction of 10-16% into the reaction kettle to adjust the pH value, sealing the reaction kettle, raising the temperature in the reaction kettle to 160-180 ℃, and reacting at high temperature for 100-120 min to prepare a thermal reactant.
2. The method for preparing a heat-resistant rubber adhesive according to claim 1, wherein the method comprises the following steps: preferably, the self-made bonding product is 8-10 parts by weight, the polyisocyanate adhesive is 30-35 parts by weight, and the chloroprene rubber is 20-24 parts by weight.
3. The method for preparing a heat-resistant rubber adhesive according to claim 1, wherein the method comprises the following steps: preferably, the weight parts of the prefabricated product are 40-42 parts, 2-4 parts of zinc oxide, 8-10 parts of methyl methacrylate and 3-5 parts of acetone.
4. The method for preparing a heat-resistant rubber adhesive according to claim 1, wherein the method comprises the following steps: the mass ratio of the hot reactant to the silicon dioxide powder in the specific preparation step (1) of the self-made bonding product is 15: 1.
5. The method for preparing a heat-resistant rubber adhesive according to claim 1, wherein the method comprises the following steps: the mass ratio of the prefabricated mixed liquid to the aluminum chloride in the specific preparation step (2) of the self-made bonding product is 30: 1.
6. The method for preparing a heat-resistant rubber adhesive according to claim 1, wherein the method comprises the following steps: the reaction liquid to be subjected to enzymolysis and the pepsin in the specific preparation step (2) of the self-made bonding product are 15:1 in mass ratio.
7. The method for preparing a heat-resistant rubber adhesive according to claim 1, wherein the method comprises the following steps: the mass ratio of the soybean flour to the soybean straw in the specific preparation step (1) of the hot reactant is 1: 10.
8. The method for preparing a heat-resistant rubber adhesive according to claim 1, wherein the method comprises the following steps: the mass ratio of the mixed material to the deionized water in the specific preparation step (1) of the thermal reactant is 1: 5.
9. The method for preparing a heat-resistant rubber adhesive according to claim 1, wherein the method comprises the following steps: the pH value of the dropwise added sodium hydroxide solution with the mass fraction of 10-16% is further preferably adjusted to be 12-13 in the specific preparation step (2) of the thermal reactant.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111363496A (en) * | 2020-04-26 | 2020-07-03 | 芜湖风雪橡胶有限公司 | Rubber adhesive and preparation method thereof |
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| WO2006102809A1 (en) * | 2005-03-31 | 2006-10-05 | Shouhui Zhu | Method for applying polymeric adhesive as adhesive agent to bond wood or garnish |
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| WO2006102809A1 (en) * | 2005-03-31 | 2006-10-05 | Shouhui Zhu | Method for applying polymeric adhesive as adhesive agent to bond wood or garnish |
| CN101255317A (en) * | 2008-04-03 | 2008-09-03 | 浙江东南橡胶机带有限公司 | High-strength thermoresistance adhesive for transmission belt and method of use thereof |
| CN109879634A (en) * | 2019-02-28 | 2019-06-14 | 江苏长龙国际贸易有限公司 | A kind of preparation method of waterproof compacting agent |
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