AU2021102582A4 - Method for synthesizing adhesive - Google Patents

Method for synthesizing adhesive Download PDF

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Publication number
AU2021102582A4
AU2021102582A4 AU2021102582A AU2021102582A AU2021102582A4 AU 2021102582 A4 AU2021102582 A4 AU 2021102582A4 AU 2021102582 A AU2021102582 A AU 2021102582A AU 2021102582 A AU2021102582 A AU 2021102582A AU 2021102582 A4 AU2021102582 A4 AU 2021102582A4
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starch
adhesive
solution
weighing
reaction mixture
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AU2021102582A
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Xiaojun Huang
Lin Liu
Xiaoguang Wang
Zishuang WANG
Faming XIA
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Wuhan Textile University
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Wuhan Textile University
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J151/00Adhesives based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Adhesives based on derivatives of such polymers
    • C09J151/02Adhesives based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Adhesives based on derivatives of such polymers grafted on to polysaccharides
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08BPOLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B30/00Preparation of starch, degraded or non-chemically modified starch, amylose, or amylopectin
    • C08B30/12Degraded, destructured or non-chemically modified starch, e.g. mechanically, enzymatically or by irradiation; Bleaching of starch
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F251/00Macromolecular compounds obtained by polymerising monomers on to polysaccharides or derivatives thereof

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Biochemistry (AREA)
  • Materials Engineering (AREA)
  • Adhesives Or Adhesive Processes (AREA)

Abstract

OF THE DISCLOSURE The present disclosure relates to a method for synthesizing a degradable adhesive. The method for synthesizing a degradable adhesive includes the following steps: step 1, placing and irradiating starch in a radiation field under aerobic conditions, to obtain a peroxide-containing pre-irradiated starch; step 2, based on 50%-200% of the mass of the pre-irradiated starch, weighing an allyl containing monomer, mixing a part thereof with the above starch solution; step 3, heating to 51 59°C, and stirring for 30 min; step 4, based on 1%o of the amount of the starch, weighing and dissolving a reducing agent in a small amount of deionized water; step 5, after dropping, keeping stirring for 10 min; step 6, based on 2-4%o of the amount of the starch, weighing and dissolving a terminator in a small amount of deionized water, adding a resulting terminator solution to the reaction mixture in one portion; and step 7, neutralizing the reaction mixture to approximately pH 5 with NaOH solution to obtain a pasty and sticky liquid, namely, a degradable adhesive. The method is characterized by simple process, low cost, high biodegradability of the adhesive obtained finally, and no secondary environmental pollution.

Description

METHOD FOR SYNTHESIZING ADHESIVE TECHNICAL FIELD
[01] The present disclosure relates to the technical field of natural organic polymer adhesives, and in particular to a method for synthesizing an adhesive.
BACKGROUNDART
[02] Adhesive, as an organic polymer, has increasingly been used widely in the fields of packaging, printing, construction engineering, textile printing and dyeing, shoemaking, and biomedicine, and has become an essential material in modern industry and national defense industry. With the rapid economic development of China, adhesives are playing more and more important roles in promoting different industries to simplify processing, saving energy, reducing costs, and improving economic performance; however, hazardous substances in the adhesives, such as volatile organic compounds, toxic curing agents, plasticizers, diluents, and other additives and harmful fillers, create new pollution and safety problems to the environment. At present, green environmental protection, resource conservation, and sustainable development are increasingly concerned all around the world, and in China, green economy is even regarded as the main development trend in the future. In view of this, adhesives widely used in packaging materials are bound to face higher environmental protection requirements. Facing increasingly stringent environmental protection requirements in the market, all adhesive manufacturers are actively looking for a way to develop, and thus degradable adhesives are becoming very popular. Active research and development of degradable energy-saving adhesives, as well as vigorous research and development of critical materials and high-performance and high-quality additives of the degradable adhesives, will become the inevitable course for the development of adhesives.
SUMMARY
[03] An objective of the present disclosure is to provide a method for synthesizing an adhesive; the method features simple process, less investment, and low cost, and can obtain an excellent adhesive effect.
[04] To achieve the above objective, the technical solution adopted by the present disclosure is: a method for synthesizing an adhesive, including the following steps:
[05] step 1, placing starch in a radiation field, and degrading the starch by irradiating at an irradiation dose of 2-100 kGy under aerobic conditions, to obtain a peroxide-containing pre irradiated starch;
[06] step 2, mixing the foregoing starch with a 0.25 mol/L acid solution in a mass ratio of 1:4 for -50 min;
[07] step 3, based on 50%-200% of the mass of the pre-irradiated starch, weighing an allyl containing monomer, mixing a part thereof with the above starch solution, heating to 51-59°C, and stirring for 30 min;
[08] step 4, based on 1%o of the amount of the starch, weighing and dissolving a reducing agent in a small amount of deionized water;
[09] step 5, dropping the remaining monomer and the reducing agent into the starch solution in step 3 simultaneously, where the dropping lasts for 1-2.5 h, and a reaction mixture is controlled at a temperature not exceeding 65°C;
[10] step 6, after dropping, keeping stirring for 10 min; and
[11] step 7, based on 2-4%o of the amount of the starch, weighing and dissolving a terminator in a small amount of deionized water, adding a resulting terminator solution to the reaction mixture in one portion, stirring for 10-20 min to terminate the reaction, and neutralizing the reaction mixture to approximately pH 5 with NaOH solution to obtain a pasty and sticky liquid, namely, a degradable adhesive.
[12] Preferably, the starch in step 1 may be any one from the group consisting of wheat starch, potato starch, cassava starch, kudzu starch, and sweet potato starch; the radiation field may be any one of y-ray, X-ray, and electron beam; acrylate in step 3 may be any one from the group consisting of butyl methacrylate, methacryloyloxyethyl trimethyl ammonium chloride, and acryloyloxyethyl trimethyl ammonium chloride; the reducing agent may be a redox system composed of ammonium persulfate and sodium sulfite.
[13] A natural organic polymer adhesive of the present disclosure may be applicable to the fields of packaging, printing, construction engineering, textile printing and dyeing, shoemaking, and biomedicine.
[14] The disclosure has the following beneficial effects: natural polymers are physically modified by a radiation method; the method is characterized by simple process, less investment, low cost, high biodegradability of the adhesive obtained finally, proneness to biodegradation, and no secondary environmental pollution.
DETAILED DESCRIPTION OF THE EMBODIMENTS
[15] The present disclosure will be further described in conjunction with specific examples. It should be understood that these examples are only intended to illustrate the present disclosure and not to limit the scope of the present disclosure. Furthermore, it should be appreciated that those skilled in the art may alter or modify the efforts of the present disclosure after reading the teachings of the present disclosure, and these equivalent forms also fall within the scope as defined by the appended claims of the present application.
[16] Example 1:
[17] A method for synthesizing an adhesive included the following steps:
[18] step 1, starch (wheat starch, viscosity 42 mp-s, moisture content 1 4 .09wt%) was placed in a y- 6 Co radiation field, and degraded by irradiating at an irradiation dose of 30 kGy under aerobic conditions (for example, in the presence of air), to obtain a peroxide-containing pre-irradiated starch;
[19] step 2, the foregoing starch was mixed with a 0.25 mol/L acid solution in a mass ratio of 1:4 for 40-50 min;
[20] step 3, based on 80% of the mass of the pre-irradiated starch, an allyl-containing monomer was weighed; a part thereof was mixed with the above starch solution, heated to 51-59°C, and stirred for 30 min;
[21] step 4, based on 1%o of the amount of the starch, a reducing agent was weighed and dissolved in a small amount of deionized water;
[22] step 5, the remaining monomer and the reducing agent were dropped into the starch solution in step 3 simultaneously, where dropping time was 1-2.5 h, and a reaction mixture was controlled at a temperature not exceeding 65°C;
[23] step 6, after dropping, stirring continued for 10 min; and
[24] step 7, based on 4%o of the amount of the starch, a terminator was weighed and dissolved in a small amount of deionized water, a resulting terminator solution was added to the reaction mixture in one portion and stirred for 10-20 min to terminate the reaction, and the reaction mixture was neutralized to approximately pH 5 with NaOH solution to obtain a pasty and sticky liquid, namely, a degradable adhesive.
[25] The resulting starch adhesive had excellent adhesive effects on paper products, plastic products, and wood products; in addition, biodegradability evaluation of the adhesive by the aerobic respiration parameter method concluded that the five-day biochemical oxygen demand (BOD5)/chemical oxygen demand (CODCr) ratio of the starch adhesive was 0.42, with better biodegradability.
[26] Example 2:
[27] A method for synthesizing an adhesive included the following steps:
[28] step 1, starch (potato starch, viscosity 49 mp-s, moisture content 13.51wt%) was placed in a y-6 Co radiation field, and degraded by irradiating at an irradiation dose of 50 kGy under aerobic conditions (for example, in the presence of air), to obtain a peroxide-containing pre-irradiated starch;
[29] step 2, the foregoing starch was mixed with a 0.25 mol/L acid solution in a mass ratio of 1:4 for 40-50 min;
[30] step 3, based on 100% of the mass of the pre-irradiated starch, an allyl-containing monomer was weighed; a part thereof was mixed with the above starch solution, heated to 51-59°C, and stirred for 30 min;
[31] step 4, based on 1%o of the amount of the starch, a reducing agent was weighed and dissolved in a small amount of deionized water;
[32] step 5, the remaining monomer and the reducing agent were dropped into the starch solution in step 3 simultaneously, where dropping time was 1-2.5 h, and a reaction mixture was controlled at a temperature not exceeding 65°C;
[33] step 6, after dropping, stirring continued for 10 min; and
[34] step 7, based on 2%o of the amount of the starch, a terminator was weighed and dissolved in a small amount of deionized water, a resulting terminator solution was added to the reaction mixture in one portion and stirred for 10-20 min to terminate the reaction, and the reaction mixture was neutralized to approximately pH 5 with NaOH solution to obtain a pasty and sticky liquid, namely, a degradable adhesive.
[35] The resulting starch adhesive had excellent adhesive effects on paper products, plastic products, and wood products; in addition, biodegradability evaluation of the adhesive by the aerobic respiration parameter method concluded that the BOD5/CODCr ratio of the starch adhesive was 0.44, with better biodegradability.
[36] Example 3:
[37] A method for synthesizing an adhesive included the following steps:
[38] step 1, starch (potato starch, viscosity 49 mp-s, moisture content 13.51wt%) was placed in an electron beam radiation field, and degraded by irradiating at an irradiation dose of 20 kGy under aerobic conditions (for example, in the presence of air), to obtain a peroxide-containing pre irradiated starch;
[39] step 2, the foregoing starch was mixed with a 0.25 mol/L acid solution in a mass ratio of 1:4 for 40-50 min;
[40] step 3, based on 120% of the mass of the pre-irradiated starch, an allyl-containing monomer was weighed; a part thereof was mixed with the above starch solution, heated to 51-59°C, and stirred for 30 min;
[41] step 4, based on 1%o of the amount of the starch, a reducing agent was weighed and dissolved in a small amount of deionized water;
[42] step 5, the remaining monomer and the reducing agent were dropped into the starch solution in step 3 simultaneously, where dropping time was 1-2.5 h, and a reaction mixture was controlled at a temperature not exceeding 65°C;
[43] step 6, after dropping, stirring continued for 10 min; and
[44] step 7, based on 4%o of the amount of the starch, a terminator was weighed and dissolved in a small amount of deionized water, a resulting terminator solution was added to the reaction mixture in one portion and stirred for 10-20 min to terminate the reaction, and the reaction mixture was neutralized to approximately pH 5 with NaOH solution to obtain a pasty and sticky liquid, namely, a degradable adhesive.
[45] The resulting starch adhesive had excellent adhesive effects on paper products, plastic products, and wood products; in addition, biodegradability evaluation of the adhesive by the aerobic respiration parameter method concluded that the BOD5/CODCr ratio of the starch adhesive was 0.45, with better biodegradability.
[46] Other types of starch can also be achieved by the present disclosure and are not elaborated herein. All raw materials and upper and lower limits thereof, along with upper and lower limits of all process parameters, listed by the present disclosure can achieve the present disclosure, and examples will not be enumerated herein.

Claims (2)

WHAT IS CLAIMED IS:
1. A method for synthesizing an adhesive, comprising the following steps: step 1, placing starch in a radiation field, and degrading the starch by irradiating at an irradiation dose of 2-100 kGy under aerobic conditions, to obtain a peroxide-containing pre irradiated starch; step 2, mixing the foregoing starch with a 0.25 mol/L acid solution in a mass ratio of 1:4 for -50 min; step 3, based on 50%-200% of the mass of the pre-irradiated starch, weighing an allyl containing monomer, mixing a part thereof with the above starch solution, heating to 51-59°C, and stirring for 30 min; step 4, based on 1%o of the amount of the starch, weighing and dissolving a reducing agent in a small amount of deionized water; step 5, dropping the remaining monomer and the reducing agent into the starch solution in step 3 simultaneously, wherein the dropping lasts for 1-2.5 h, and a reaction mixture is controlled at a temperature not exceeding 65°C; step 6, after dropping, keeping stirring for 10 min; and step 7, based on 2-4%o of the amount of the starch, weighing and dissolving a terminator in a small amount of deionized water, adding a resulting terminator solution to the reaction mixture in one portion, stirring for 10-20 min to terminate the reaction, and neutralizing the reaction mixture to approximately pH 5 with NaOH solution to obtain a pasty and sticky liquid, namely, a degradable adhesive.
2. The method for synthesizing an adhesive according to claim 1, wherein, the starch in step 1 is any one from the group consisting of potato starch, cassava starch, kudzu starch, and sweet potato starch; the radiation field is any one of y-ray, X-ray, and electron beam; acrylate in step 3 is any one from the group consisting of butyl meth acrylate, methacryloyloxyethyl trimethyl ammonium chloride, and acryloyloxyethyl trimethyl ammonium chloride; the reducing agent is a redox system comprising ammonium persulfate and sodium sulfite.
AU2021102582A 2021-05-14 2021-05-14 Method for synthesizing adhesive Ceased AU2021102582A4 (en)

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