CN111100560A - Preparation method of waterproof heat-resistant cigarette adhesive - Google Patents
Preparation method of waterproof heat-resistant cigarette adhesive Download PDFInfo
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- CN111100560A CN111100560A CN201911288749.XA CN201911288749A CN111100560A CN 111100560 A CN111100560 A CN 111100560A CN 201911288749 A CN201911288749 A CN 201911288749A CN 111100560 A CN111100560 A CN 111100560A
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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
- 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
Abstract
The invention discloses a preparation method of a waterproof heat-resistant cigarette adhesive, and belongs to the technical field of adhesive preparation. Mixing straws and starch, performing hydrochloric acid soaking, sodium hypochlorite oxidation, high-temperature high-pressure reaction and amylase enzymolysis to decompose the straws and the starch, extracting fiber components, decomposing the starch to generate sugar components with smaller molecular weight, such as maltose, and the like, and utilizing bonds such as hydrogen bonds formed by abundant hydroxyl groups in the sugar and other components in the cigarette adhesive to generate adsorption, so that bonding effect is formed between fiber molecules and the surrounding components, and the structural strength of the cigarette adhesive is improved; according to the invention, silicon dioxide is introduced into organic components such as fiber components, sugar components and the like, the organic components are decomposed by utilizing the high-temperature and high-pressure reaction of alkali liquor, and simultaneously, silicon dioxide molecules are hydrolyzed to generate silicate components, so that silicate is adsorbed in the organic fibers through ionic bonds and electrostatic ions, and the water resistance of the cigarette adhesive is improved by utilizing the good thermal stability and hydrophobic property of the cigarette adhesive.
Description
Technical Field
The invention discloses a preparation method of a waterproof heat-resistant cigarette adhesive, and belongs to the technical field of adhesive preparation.
Background
The cigarette adhesive comprises lap adhesive, joint adhesive and packaging adhesive, and plays an important role in cigarette rolling, packaging quality and cigarette internal quality although the consumption of the cigarette adhesive is small in the cigarette production process. The particularity of the cigarette production process determines that the cigarette adhesive becomes a special adhesive. Firstly, the type selection must be adapted to the requirements of spraying or rolling of the wrapping machine, the drying speed also needs to be adapted to the requirements of high-speed production of the machine, and better material adaptability is needed. Secondly, the cigarette adhesive needs to have higher stability, and can stably and cleanly run on a machine for a long time, so that the operation and the production efficiency of the cigarette machine are greatly influenced. The quality of cigarette glue greatly affects the quality level of cigarettes. The cigarette adhesive needs to have good bonding strength and fluidity, the drying speed of the cigarette adhesive also needs to be adapted to the standard of high-speed production of cigarette making machines, and the cigarette adhesive needs to have longer storage period and stability and has better adaptability to cigarette equipment.
In the cigarette adhesive, the lap adhesive directly participates in cigarette combustion, the mouthpiece adhesive is directly contacted with the mouth of a person, and the using amount of the both is larger, so that the influence of the quality on the quality of cigarette products and smoking safety is more worthy of attention than other adhesive varieties. Along with the improvement of the attention degree of people on the smoking safety of cigarettes, the requirements of cigarette enterprises on raw materials, production processes and cigarette glue are higher and higher. The 2004 national tobacco agency sets forth an industry standard for high speed cigarette glue, wherein it is pointed out that the maximum amount of residual monomer is 0.5%, but no regulations are made for the types of auxiliary materials and monomers except for precious metals (calculated as lead) and toxic metals (calculated as arsenic). The cigarette industry in 2010 updates standards (MK/JS 517-2010), and increases indexes of contents of benzene, toluene, xylene, phthalate, formaldehyde and vinyl acetate (namely vinyl acetate, or vinyl acetate and vinyl acetate), wherein the content of vinyl acetate monomer residues is less than 1000 mg/kg. In 2012, there was a requirement from cigarette factories to reduce the residual vinyl acetate monomer content to 350 mg/kg.
With the increasing awareness of environmental protection and the stricter requirements on the content of volatile organic compounds in the adhesive, the preparation of cigarette adhesives from natural materials is a necessary trend. The starch has wide sources and is green and environment-friendly, has a long history of being used as an adhesive, is a renewable natural high polymer material, and is one of the most potential natural materials for replacing petrochemical raw materials. Are used industrially as textile sizing agents, corrugated board adhesives and paper sizing agents. The starch has good bonding performance and attracts people's attention as the base material of the cigarette adhesive, but the poor heat resistance of the existing cigarette adhesive causes the viscosity of the cigarette adhesive to be reduced under the heating condition, and meanwhile, the poor waterproof performance of the cigarette adhesive is a key factor for restricting the development of the cigarette adhesive. With the progress of science and technology and the continuous and deep research, the starch adhesive is used as a natural renewable environment-friendly material to replace a synthetic adhesive to be used as a cigarette adhesive, and the development trend is certainly reached.
Chinese patent CN102181243A synthesizes ternary copolymer emulsion from vinyl acetate, butyl acrylate and acrylic acid ternary monomers under the action of ammonium persulfate-sodium bisulfite composite initiator, and finally adds plasticizer and vacuumizes. Yanlixin, in the research and development of corn starch modified high-speed cigarette lap adhesive, mentions that corn starch, sodium hypochlorite and borax are oxidized, then are subjected to grafting reaction with PVA, then VAE707 and an emulsifier are added for carrying out an emulsification reaction, a monomer and an initiator are added, the heat preservation reaction is carried out, and finally the cigarette lap adhesive is obtained by filtering. However, the method still mainly uses polyvinyl acetate, and is not real starch cigarette glue; and the defects of the existing cigarette adhesive are not solved.
Therefore, the invention of the cigarette adhesive with good heat resistance and water 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 viscosity of the cigarette adhesive is reduced under the heating condition caused by poor heat resistance of the existing cigarette adhesive and the waterproof performance of the cigarette adhesive is poor, the preparation method of the waterproof heat-resistant cigarette adhesive is provided.
In order to solve the technical problems, the invention adopts the technical scheme that:
a preparation method of the waterproof heat-resistant cigarette adhesive comprises the following steps:
putting the modified binder, benzoic acid, carboxymethyl cellulose, ammonium persulfate, methyl acrylate and a cigarette adhesive blank into a stirring kettle, raising the temperature in the stirring kettle to 45-50 ℃, stirring for 1-2 hours at the rotating speed of 300-400 r/min by using a stirrer, raising the temperature in the reaction kettle to 70-80 ℃ after stirring, continuing stirring for 50-60 minutes, and discharging after stirring to obtain the waterproof heat-resistant cigarette adhesive;
the specific preparation steps of the modified binder are as follows:
putting a reaction binder and silicon dioxide into a reaction kettle, dropwise adding a sodium hydroxide solution with the mass fraction of 10-15% into the reaction kettle to adjust the pH value to be only 11-12, sealing the reaction kettle, raising the air pressure in the reaction kettle to 1.2-1.5 MPa, raising the temperature in the reaction kettle to 160-180 ℃ under the constant pressure condition, carrying out constant-temperature and constant-pressure reaction for 40-60 min, dropwise adding a sulfuric acid solution with the mass fraction of 10-15% after the reaction to adjust the pH value to 6.0-6.5, and continuously heating for 2-3 h under the temperature of 80-100 ℃ after the adjustment to obtain a modified binder;
the reaction binder is prepared by the following specific steps:
(1) putting corn straws and corn starch into a crusher to be crushed and mixed to obtain a mixed material, putting the mixed material and hydrochloric acid with the mass fraction of 10-15% into a beaker, stirring for 50-60 min at the rotating speed of 300-400 r/min by using a stirrer, putting the beaker into an ultrasonic oscillator after stirring, and oscillating for 2-3 h under the condition of the frequency of 32-36 kHz to prepare mixed slurry;
(2) adding sodium hypochlorite powder into a beaker, placing the beaker into a water bath kettle with a water bath temperature of 35-45 ℃, stirring for 50-60 min at a rotating speed of 400-500 r/min by using a stirring device, preparing an oxidation mixture after stirring, and dropwise adding a sulfuric acid solution with the mass fraction of 60-80% into the beaker to prepare an acidic reaction solution;
(3) sealing the beaker in a resistance heating sleeve, raising the temperature in the heating sleeve to 60-70 ℃, heating at a constant temperature for 60-80 min, dropwise adding a sodium hydroxide solution with the mass fraction of 6-10% into the beaker after heating to adjust the pH value, stirring for 40-60 min at the rotating speed of 1000-1200 r/min by using a stirring device, putting the materials in the beaker into a rotary evaporator after stirring, and concentrating for 2-3 h under the conditions of the rotating speed of 250-270 r/min and the temperature of 50-60 ℃ to obtain a concentrated product;
(4) putting the concentrated product, sodium citrate, potassium chloride, amylase and distilled water into an enzymolysis tank, putting the enzymolysis tank into a greenhouse with the indoor temperature of 32-36 ℃, standing at a constant temperature for 5-6 h, heating, putting into a reaction kettle, raising the temperature in the reaction kettle to 90-100 ℃, and heating at the constant temperature for 40-50 min to obtain the reaction binder.
Preferably, the modified binder comprises, by weight, 12-15 parts of benzoic acid, 1.0-1.2 parts of carboxymethyl cellulose, 1-2 parts of ammonium persulfate, 10-12 parts of methyl acrylate and 40-45 parts of cigarette rubber blank.
The mass ratio of the reactive binder to the silica in the specific preparation step of the modified binder is 20: 1.
The mass ratio of the corn stalks to the corn starch in the specific preparation step (1) of the reaction binder is 10: 1.
The mass ratio of the mixed material and hydrochloric acid with the mass fraction of 10-15% in the specific preparation step (1) of the reaction binder is 1: 5.
The mass of the sodium hypochlorite powder added into the beaker in the concrete preparation step (2) of the reaction binder is 3-5% of the mass of the mixed slurry.
Specifically, the mass of the acidic reaction solution prepared by dropwise adding a 60-80% sulfuric acid solution into the beaker in the step (2) of preparing the reaction binder is 15-20% of the mass of the oxidation mixture.
The pH value is further preferably 6.5-7.0 by adding a sodium hydroxide solution with the mass fraction of 6-10% dropwise in the specific preparation step (3) of the reaction binder.
In the specific preparation step (4) of the reaction binder, the preferable weight portions include 12-14 parts of concentrated product, 1.0-1.2 parts of sodium citrate, 1.2-1.5 parts of potassium chloride, 0.6-0.8 part of amylase and 6-8 parts of distilled water.
The beneficial technical effects of the invention are as follows:
(1) the invention firstly crushes and mixes the corn stalk and the corn starch, mixes them, soaks and oscillates with hydrochloric acid to produce mixed slurry, adds sodium hypochlorite into the mixed slurry to react, adds sulphuric acid to produce acid reaction liquid after reaction, then heats the acid reaction liquid, adds alkali liquor to adjust the pH value after heating, and then concentrates to produce concentrated product after adjusting the pH value, then mixes the concentrated product with amylase and other auxiliary agents to carry out enzymolysis reaction, heats them to produce reaction binder after reaction, then mixes the reaction binder with silicon dioxide, reacts at high temperature and high pressure in the alkali liquor environment, adjusts the pH value after reaction and heats them to produce modified binder, finally heats and stirs the modified binder, the cigarette glue blank and other auxiliary agents, and discharges them to produce the waterproof and heat-resistant cigarette glue. Straw and starch are decomposed, fiber components are extracted, the starch is decomposed to generate sugar components with smaller molecular weight, such as maltose, and the like, and the adsorption effect is generated by utilizing bonds such as hydrogen bonds formed by rich hydroxyl groups contained in the sugar and other components in the cigarette adhesive, so that the bonding effect is formed between fiber molecules and all the surrounding components, and the cigarette adhesive is solidified to form a cross-linked structure in the cigarette adhesive through the fiber components, so that the structural strength of the cigarette adhesive is improved, the viscosity of the cigarette adhesive after solidification is enhanced, and the structural strength is increased, so that the space between all the molecules in the cigarette adhesive after solidification is shortened, and the waterproof and anti-permeation performance of the cigarette adhesive is improved;
(2) according to the invention, silicon dioxide is introduced into organic components such as fiber components, sugar components and the like, alkali liquor is utilized to react at high temperature and high pressure to decompose the organic components and hydrolyze silicon dioxide molecules to generate silicate components, so that silicate is adsorbed in the organic fibers through ionic bonds and electrostatic ions, the pH value is adjusted and the silicate is heated to react to generate silicon dioxide nano-scale particles which are bonded in the fiber components, the fiber components and the organic components are coated to play a protective role, the water resistance of the cigarette adhesive is improved by utilizing the good thermal stability and hydrophobic property of the cigarette adhesive, the heat resistance of the cigarette adhesive is improved, and the cigarette adhesive has a wide application prospect.
Detailed Description
Putting corn straws and corn starch into a grinder according to the mass ratio of 10:1 for grinding and mixing to obtain a mixed material, putting the mixed material and 10-15% hydrochloric acid according to the mass ratio of 1:5 into a beaker, stirring for 50-60 min at the rotating speed of 300-400 r/min by using a stirrer, putting the beaker into an ultrasonic oscillator after stirring, and oscillating for 2-3 h under the condition of the frequency of 32-36 kHz to obtain mixed slurry; adding sodium hypochlorite powder accounting for 3-5% of the mass of the mixed slurry into the beaker, placing the beaker into a water bath kettle with the water bath temperature of 35-45 ℃, stirring for 50-60 min at the rotating speed of 400-500 r/min by using a stirring device, preparing an oxidation mixture after stirring, and dropwise adding a sulfuric acid solution accounting for 15-20% of the mass of the oxidation mixture and accounting for 60-80% of the mass of the oxidation mixture into the beaker to prepare an acidic reaction solution; sealing the beaker in a resistance heating sleeve, raising the temperature in the heating sleeve to 60-70 ℃, heating at a constant temperature for 60-80 min, dropwise adding a sodium hydroxide solution with the mass fraction of 6-10% into the beaker after heating to adjust the pH value to 6.5-7.0, stirring for 40-60 min by using a stirring device at the rotating speed of 1000-1200 r/min, putting the materials in the beaker into a rotary evaporator after stirring, and concentrating for 2-3 h under the conditions of the rotating speed of 250-270 r/min and the temperature of 50-60 ℃ to obtain a concentrated product; according to the weight parts, 12-14 parts of the concentrated product, 1.0-1.2 parts of sodium citrate, 1.2-1.5 parts of potassium chloride, 0.6-0.8 part of amylase and 6-8 parts of distilled water are put into an enzymolysis tank, the enzymolysis tank is placed in a greenhouse with the indoor temperature of 32-36 ℃, the enzymolysis tank is kept stand at a constant temperature for 5-6 hours, the enzymolysis tank is put into a reaction kettle after being heated, the temperature in the reaction kettle is raised to 90-100 ℃, and the reaction binder is prepared by heating at the constant temperature for 40-50 min; putting the reaction binder and silicon dioxide into a reaction kettle according to a mass ratio of 20:1, dropwise adding a sodium hydroxide solution with a mass fraction of 10-15% into the reaction kettle to adjust the pH value to be only 11-12, sealing the reaction kettle, raising the air pressure in the reaction kettle to 1.2-1.5 MPa, raising the temperature in the reaction kettle to 160-180 ℃ under a constant pressure condition, carrying out constant-temperature and constant-pressure reaction for 40-60 min, dropwise adding a sulfuric acid solution with a mass fraction of 10-15% after the reaction to adjust the pH value to 6.0-6.5, and continuously heating for 2-3 h under a temperature of 80-100 ℃ after the adjustment to obtain a modified binder; according to the weight parts, 12-15 parts of the modified binder, 1.0-1.2 parts of benzoic acid, 0.5-0.7 part of carboxymethyl cellulose, 1-2 parts of ammonium persulfate, 10-12 parts of methyl acrylate and 40-45 parts of a cigarette adhesive blank are put into a stirring kettle, the temperature in the stirring kettle is raised to 45-50 ℃, the stirring kettle is used for stirring for 1-2 hours at the rotating speed of 300-400 r/min, the temperature in the reaction kettle is raised to 70-80 ℃ after stirring, stirring is continued for 50-60 minutes, and the waterproof heat-resistant cigarette adhesive is obtained after discharging after stirring.
Example 1
Preparation of an acidic reaction solution:
putting corn straws and corn starch into a crusher according to the mass ratio of 10:1 to be crushed and mixed to obtain a mixed material, putting the mixed material and 10% hydrochloric acid according to the mass ratio of 1:5 into a beaker, stirring for 50min at the rotating speed of 300r/min by using a stirrer, putting the beaker into an ultrasonic oscillator after stirring, and oscillating for 2h under the condition of the frequency of 32kHz to obtain mixed slurry;
adding sodium hypochlorite powder accounting for 3% of the mass of the mixed slurry into the beaker, placing the beaker into a water bath kettle with the water bath temperature of 35 ℃, stirring for 50min at the rotating speed of 400r/min by using a stirring device, preparing an oxidation mixture after stirring, and dropwise adding a sulfuric acid solution accounting for 60% of the mass of the oxidation mixture and accounting for 15% of the mass of the oxidation mixture into the beaker to prepare an acidic reaction solution;
preparation of a reaction binder:
sealing the beaker in a resistance heating sleeve, raising the temperature in the heating sleeve to 60 ℃, heating at a constant temperature for 60min, dropwise adding a sodium hydroxide solution with the mass fraction of 6% into the beaker after heating to adjust the pH value to 6.5, stirring for 40min at the rotating speed of 1000r/min by using a stirring device, putting the materials in the beaker into a rotary evaporator after stirring, and concentrating for 2h under the conditions of the rotating speed of 250r/min and the temperature of 50 ℃ to obtain a concentrated product;
putting 12 parts of the concentrated product, 1.0 part of sodium citrate, 1.2 parts of potassium chloride, 0.6 part of amylase and 6 parts of distilled water into an enzymolysis tank, putting the enzymolysis tank into a greenhouse with the indoor temperature of 32 ℃, standing for 5 hours at a constant temperature, heating, putting into a reaction kettle, raising the temperature in the reaction kettle to 90 ℃, and heating at the constant temperature for 40 minutes to obtain a reaction binder;
preparing a waterproof heat-resistant cigarette adhesive:
putting the reaction binder and silicon dioxide into a reaction kettle according to the mass ratio of 20:1, dropwise adding a 10% sodium hydroxide solution into the reaction kettle to adjust the pH value to be only 11, sealing the reaction kettle, raising the air pressure in the reaction kettle to 1.2MPa, raising the temperature in the reaction kettle to 160 ℃ under the constant pressure condition, carrying out constant-temperature and constant-pressure reaction for 40min, dropwise adding a 10% sulfuric acid solution after the reaction to adjust the pH value to 6.0, and continuously heating for 2h under the temperature of 80 ℃ after the adjustment to obtain a modified binder;
according to the weight parts, 12 parts of the modified binder, 1.0 part of benzoic acid, 0.5 part of carboxymethyl cellulose, 1 part of ammonium persulfate, 10 parts of methyl acrylate and 40 parts of cigarette adhesive blank are put into a stirring kettle, the temperature in the stirring kettle is raised to 45 ℃, the stirring kettle is used for stirring for 1h at the rotating speed of 300r/min, the temperature in the reaction kettle is raised to 70 ℃ after stirring, the stirring is continued for 50min, and the waterproof heat-resistant cigarette adhesive is obtained after the discharging after the stirring.
Example 2
Preparation of an acidic reaction solution:
putting corn straws and corn starch into a grinder according to the mass ratio of 10:1 for grinding and mixing to obtain a mixed material, putting the mixed material and 11% hydrochloric acid into a beaker according to the mass ratio of 1:5, stirring for 55min at the rotating speed of 350r/min by using a stirrer, putting the beaker into an ultrasonic oscillator after stirring, and oscillating for 2.5h under the condition of the frequency of 34kHz to obtain mixed slurry;
adding sodium hypochlorite powder accounting for 4% of the mass of the mixed slurry into the beaker, placing the beaker into a water bath kettle with the water bath temperature of 40 ℃, stirring for 55min at the rotating speed of 450r/min by using a stirring device, preparing an oxidation mixture after stirring, and dropwise adding a sulfuric acid solution accounting for 17% of the mass of the oxidation mixture and accounting for 70% of the mass of the oxidation mixture into the beaker to prepare an acidic reaction solution;
preparation of a reaction binder:
sealing the beaker in a resistance heating sleeve, raising the temperature in the heating sleeve to 65 ℃, heating at a constant temperature for 70min, dropwise adding a sodium hydroxide solution with the mass fraction of 8% into the beaker after heating to adjust the pH value to 6.7, stirring for 50min at the rotating speed of 1100r/min by using a stirring device, putting the materials in the beaker into a rotary evaporator after stirring, and concentrating for 2.5h under the conditions of the rotating speed of 260r/min and the temperature of 55 ℃ to obtain a concentrated product;
putting 13 parts of the concentrated product, 1.1 parts of sodium citrate, 1.4 parts of potassium chloride, 0.7 part of amylase and 7 parts of distilled water into an enzymolysis tank, putting the enzymolysis tank into a greenhouse with an indoor temperature of 34 ℃, standing at a constant temperature for 5.5 hours, heating, putting into a reaction kettle, raising the temperature in the reaction kettle to 95 ℃, and heating at the constant temperature for 45min to obtain a reaction binder;
preparing a waterproof heat-resistant cigarette adhesive:
putting the reaction binder and silicon dioxide into a reaction kettle according to the mass ratio of 20:1, dropwise adding a sodium hydroxide solution with the mass fraction of 12% into the reaction kettle to adjust the pH value to be only 11, sealing the reaction kettle, raising the air pressure in the reaction kettle to 1.4MPa, raising the temperature in the reaction kettle to 170 ℃ under the constant pressure condition, carrying out constant-temperature and constant-pressure reaction for 50min, dropwise adding a sulfuric acid solution with the mass fraction of 12% after the reaction to adjust the pH value to 6.2, and continuously heating for 2.5h under the temperature condition of 90 ℃ after the adjustment to obtain a modified binder;
and (2) putting 14 parts of the modified binder, 1.1 part of benzoic acid, 0.6 part of carboxymethyl cellulose, 1 part of ammonium persulfate, 11 parts of methyl acrylate and 42 parts of cigarette adhesive blank into a stirring kettle, raising the temperature in the stirring kettle to 47 ℃, stirring for 1.5 hours at the rotating speed of 350r/min by using a stirrer, raising the temperature in the reaction kettle to 75 ℃ after stirring, continuing stirring for 55 minutes, and discharging after stirring to obtain the waterproof heat-resistant cigarette adhesive.
Example 3
Preparation of an acidic reaction solution:
putting corn straws and corn starch into a crusher according to the mass ratio of 10:1 to be crushed and mixed to obtain a mixed material, putting the mixed material and 15% hydrochloric acid according to the mass ratio of 1:5 into a beaker, stirring for 60min at the rotating speed of 400r/min by using a stirrer, putting the beaker into an ultrasonic oscillator after stirring, and oscillating for 3h under the condition of the frequency of 36kHz to obtain mixed slurry;
adding sodium hypochlorite powder accounting for 5% of the mass of the mixed slurry into the beaker, placing the beaker into a water bath kettle with the water bath temperature of 45 ℃, stirring for 60min at the rotating speed of 500r/min by using a stirring device, preparing an oxidation mixture after stirring, and dropwise adding a sulfuric acid solution accounting for 20% of the mass of the oxidation mixture and accounting for 80% of the mass of the oxidation mixture into the beaker to prepare an acidic reaction solution;
preparation of a reaction binder:
sealing the beaker in a resistance heating sleeve, raising the temperature in the heating sleeve to 70 ℃, heating at a constant temperature for 80min, dropwise adding a sodium hydroxide solution with the mass fraction of 10% into the beaker after heating to adjust the pH value to 7.0, stirring for 60min at the rotating speed of 1200r/min by using a stirring device, putting the materials in the beaker into a rotary evaporator after stirring, and concentrating for 3h under the conditions of the rotating speed of 270r/min and the temperature of 60 ℃ to obtain a concentrated product;
putting 14 parts of the concentrated product, 1.2 parts of sodium citrate, 1.5 parts of potassium chloride, 0.8 part of amylase and 8 parts of distilled water into an enzymolysis tank, putting the enzymolysis tank into a greenhouse with an indoor temperature of 36 ℃, standing at a constant temperature for 6 hours, heating, putting into a reaction kettle, raising the temperature in the reaction kettle to 100 ℃, and heating at the constant temperature for 50min to obtain a reaction binder;
preparing a waterproof heat-resistant cigarette adhesive:
putting the reaction binder and silicon dioxide into a reaction kettle according to the mass ratio of 20:1, dropwise adding 15% sodium hydroxide solution into the reaction kettle to adjust the pH value to be only 12, sealing the reaction kettle, raising the air pressure in the reaction kettle to 1.5MPa, raising the temperature in the reaction kettle to 180 ℃ under the constant pressure condition, carrying out constant-temperature and constant-pressure reaction for 60min, dropwise adding 15% sulfuric acid solution after the reaction to adjust the pH value to 6.5, and continuously heating for 3h under the temperature of 100 ℃ after the adjustment to obtain the modified binder;
and (2) putting 15 parts of the modified binder, 1.2 parts of benzoic acid, 0.7 part of carboxymethyl cellulose, 2 parts of ammonium persulfate, 12 parts of methyl acrylate and 45 parts of cigarette adhesive blank into a stirring kettle, raising the temperature in the stirring kettle to 50 ℃, stirring for 2 hours at a rotating speed of 400r/min by using a stirrer, raising the temperature in the reaction kettle to 80 ℃ after stirring, continuing stirring for 60 minutes, and discharging after stirring to obtain the waterproof heat-resistant cigarette adhesive.
Comparative example 1: the procedure was essentially the same as in example 2 except that the acidic reaction solution was absent.
Comparative example 2: essentially the same procedure as in example 2 was followed except that the reactive binder was absent.
Comparative example 3: a waterproof heat-resistant cigarette adhesive produced by Shandong company.
Heat resistance viscosity test: the emulsion was measured with a model NDJ-1 rotational viscometer as described in GB/T2794-1995. The test temperature was 60. + -. 0.5 ℃.
And (3) testing the waterproofness: the cigarette glues of the examples and comparative examples were used for carton packaging and the viscosity was measured after rinsing them 10 times with water.
Table 1: cigarette adhesive property measurement results
| Detecting items | Example 1 | Example 2 | Example 3 | Comparative example 1 | Comparative example 2 | Comparative example 3 |
| Heat resistance viscosity (mpa. s) | 942 | 950 | 960 | 620 | 610 | 642 |
| Water resistance viscosity (mpa. s) | 801 | 813 | 820 | 513 | 526 | 541 |
In summary, it can be seen from table 1 that the cigarette adhesive of the present invention has good heat resistance, high viscosity under heating, good water resistance, and broad 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 waterproof heat-resistant cigarette adhesive is characterized by comprising the following specific preparation steps:
putting the modified binder, benzoic acid, carboxymethyl cellulose, ammonium persulfate, methyl acrylate and a cigarette adhesive blank into a stirring kettle, raising the temperature in the stirring kettle to 45-50 ℃, stirring for 1-2 hours at the rotating speed of 300-400 r/min by using a stirrer, raising the temperature in the reaction kettle to 70-80 ℃ after stirring, continuing stirring for 50-60 minutes, and discharging after stirring to obtain the waterproof heat-resistant cigarette adhesive;
the specific preparation steps of the modified binder are as follows:
putting a reaction binder and silicon dioxide into a reaction kettle, dropwise adding a sodium hydroxide solution with the mass fraction of 10-15% into the reaction kettle to adjust the pH value to be only 11-12, sealing the reaction kettle, raising the air pressure in the reaction kettle to 1.2-1.5 MPa, raising the temperature in the reaction kettle to 160-180 ℃ under the constant pressure condition, carrying out constant-temperature and constant-pressure reaction for 40-60 min, dropwise adding a sulfuric acid solution with the mass fraction of 10-15% after the reaction to adjust the pH value to 6.0-6.5, and continuously heating for 2-3 h under the temperature of 80-100 ℃ after the adjustment to obtain a modified binder;
the reaction binder is prepared by the following specific steps:
(1) putting corn straws and corn starch into a crusher to be crushed and mixed to obtain a mixed material, putting the mixed material and hydrochloric acid with the mass fraction of 10-15% into a beaker, stirring for 50-60 min at the rotating speed of 300-400 r/min by using a stirrer, putting the beaker into an ultrasonic oscillator after stirring, and oscillating for 2-3 h under the condition of the frequency of 32-36 kHz to prepare mixed slurry;
(2) adding sodium hypochlorite powder into a beaker, placing the beaker into a water bath kettle with a water bath temperature of 35-45 ℃, stirring for 50-60 min at a rotating speed of 400-500 r/min by using a stirring device, preparing an oxidation mixture after stirring, and dropwise adding a sulfuric acid solution with the mass fraction of 60-80% into the beaker to prepare an acidic reaction solution;
(3) sealing the beaker in a resistance heating sleeve, raising the temperature in the heating sleeve to 60-70 ℃, heating at a constant temperature for 60-80 min, dropwise adding a sodium hydroxide solution with the mass fraction of 6-10% into the beaker after heating to adjust the pH value, stirring for 40-60 min at the rotating speed of 1000-1200 r/min by using a stirring device, putting the materials in the beaker into a rotary evaporator after stirring, and concentrating for 2-3 h under the conditions of the rotating speed of 250-270 r/min and the temperature of 50-60 ℃ to obtain a concentrated product;
(4) putting the concentrated product, sodium citrate, potassium chloride, amylase and distilled water into an enzymolysis tank, putting the enzymolysis tank into a greenhouse with the indoor temperature of 32-36 ℃, standing at a constant temperature for 5-6 h, heating, putting into a reaction kettle, raising the temperature in the reaction kettle to 90-100 ℃, and heating at the constant temperature for 40-50 min to obtain the reaction binder.
2. The preparation method of the waterproof heat-resistant cigarette adhesive according to claim 1, characterized in that: preferably, the modified binder comprises, by weight, 12-15 parts of benzoic acid, 1.0-1.2 parts of carboxymethyl cellulose, 1-2 parts of ammonium persulfate, 10-12 parts of methyl acrylate and 40-45 parts of cigarette rubber blank.
3. The preparation method of the waterproof heat-resistant cigarette adhesive according to claim 1, characterized in that: the mass ratio of the reactive binder to the silica in the specific preparation step of the modified binder is 20: 1.
4. The preparation method of the waterproof heat-resistant cigarette adhesive according to claim 1, characterized in that: the mass ratio of the corn stalks to the corn starch in the specific preparation step (1) of the reaction binder is 10: 1.
5. The preparation method of the waterproof heat-resistant cigarette adhesive according to claim 1, characterized in that: the mass ratio of the mixed material and hydrochloric acid with the mass fraction of 10-15% in the specific preparation step (1) of the reaction binder is 1: 5.
6. The preparation method of the waterproof heat-resistant cigarette adhesive according to claim 1, characterized in that: the mass of the sodium hypochlorite powder added into the beaker in the concrete preparation step (2) of the reaction binder is 3-5% of the mass of the mixed slurry.
7. The preparation method of the waterproof heat-resistant cigarette adhesive according to claim 1, characterized in that: specifically, the mass of the acidic reaction solution prepared by dropwise adding a 60-80% sulfuric acid solution into the beaker in the step (2) of preparing the reaction binder is 15-20% of the mass of the oxidation mixture.
8. The preparation method of the waterproof heat-resistant cigarette adhesive according to claim 1, characterized in that: the pH value is further preferably 6.5-7.0 by adding a sodium hydroxide solution with the mass fraction of 6-10% dropwise in the specific preparation step (3) of the reaction binder.
9. The preparation method of the waterproof heat-resistant cigarette adhesive according to claim 1, characterized in that: in the specific preparation step (4) of the reaction binder, the preferable weight portions include 12-14 parts of concentrated product, 1.0-1.2 parts of sodium citrate, 1.2-1.5 parts of potassium chloride, 0.6-0.8 part of amylase and 6-8 parts of distilled water.
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| CN201911288749.XA CN111100560A (en) | 2019-12-16 | 2019-12-16 | Preparation method of waterproof heat-resistant cigarette adhesive |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113437259A (en) * | 2021-05-17 | 2021-09-24 | 惠州市豪鹏科技有限公司 | Preparation method of lithium ion battery pole piece |
| CN114410249A (en) * | 2022-02-16 | 2022-04-29 | 连云港昌瑞科技有限公司 | Preparation method of waterproof heat-resistant cigarette adhesive |
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2019
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113437259A (en) * | 2021-05-17 | 2021-09-24 | 惠州市豪鹏科技有限公司 | Preparation method of lithium ion battery pole piece |
| CN114410249A (en) * | 2022-02-16 | 2022-04-29 | 连云港昌瑞科技有限公司 | Preparation method of waterproof heat-resistant cigarette adhesive |
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