CN104804136A - Synthetic method of degradable adhesive - Google Patents
Synthetic method of degradable adhesive Download PDFInfo
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- CN104804136A CN104804136A CN201510048816.6A CN201510048816A CN104804136A CN 104804136 A CN104804136 A CN 104804136A CN 201510048816 A CN201510048816 A CN 201510048816A CN 104804136 A CN104804136 A CN 104804136A
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Abstract
The invention relates to a synthetic method of a degradable adhesive. The synthetic method comprises following steps: 1) starch is subjected to irradiation in an aerobic irradiation field so as to obtain pre-irradiated starch; 2) a monomer containing vinyl or allyl is added into a mixture of the irradiated starch and water, wherein adding amount of the monomer accounts for 50 to 200% of the amount of the irradiated starch, an obtained mixed material is heated to 45 to 60 DEG C, and is stirred for 30min; 3) a reducing agent is weighed and dissolved in a small amount of deionized water, an obtained mixed solution is added into an obtained reactant dropwise, and after adding, an obtained mixed product is stirred continuously for 10min, wherein the amount of the reducing agent accounts for 0.1% of the amount of the deionized water; and 4) a terminating agent is weighed and dissolved in a small amount of deionized water, an obtained mixed liquid is added into an obtained mixed product in one time, and pH value of an obtained product is adjusted to about 5 with NaOH so as to obtain the degradable adhesive which is a sticky solution, wherein the amount of the terminating agent accounts for 0.2% of the amount of the deioinzed water. The synthetic method is simple; cost is relatively low; biodegradability of the degradable adhesive is high; and no secondary pollution is caused to the environment.
Description
Technical field
The invention belongs to natural organic high-molecular sizing agent technical field, particularly relate to a kind of synthetic method of degradable sizing agent.
Background technology
Sizing agent, as a kind of organic high molecular compound, obtains increasingly extensive application at neighborhoods such as packaging, printing, construction work, textile printing and dyeing, shoemaking, biological medicines, has become modern industry and the indispensable a kind of material of national defense industry.Along with the fast development of China's economy, sizing agent in promotion every profession and trade Simplified flowsheet, save energy, reduce costs, to increase the benefit etc. in play more and more important effect, but the objectionable impurities simultaneously in sizing agent, as volatile organic compounds, poisonous solidifying agent, softening agent, thinner and other auxiliary agent and harmful filler etc., also bring new pollution problem and safety problem to environment.Current countries in the world for environmental protection, economize on resources, Sustainable development pay attention to day by day, China is especially using the Main way of green economy as Future Development.To this, in wrapping material, the sizing agent of widespread use also must be faced with higher environmental requirement.In the face of the environmental requirement that increasing market is strict, development is all actively being found by each sizing agent manufacturing enterprise, and thus degradable sizing agent becomes and be much sought after.Positive research and development degradable, energy-saving sizing agent, research and develop degradable sizing agent critical material, high-performance high-quality auxiliary agent energetically simultaneously, become the only way of sizing agent development.
Summary of the invention
The object of the present invention is to provide a kind of synthetic method of degradable sizing agent, the method has that technique is simple, investment goods is few, cost is lower, and can obtain good gluing effect.
For achieving the above object, the technical solution adopted in the present invention is: a kind of synthetic method of degradable sizing agent, is characterized in that comprising the following steps:
1) starch is placed in irradiation field, under aerobic conditions, carries out irradiation, irradiation dose 2 ~ 100 kGy, makes it degrade, and obtains the pre-irradiation starch containing superoxide;
2) by the acid solution combination treatment 10 ~ 60 minutes of above-mentioned the starch ratio of 1:10 and 0.1mol/L in mass ratio;
3) measure the monomer containing vinyl or allylic by 50% ~ 200% of pre-irradiation starch quality, get wherein a part and above-mentioned starch liquid mixing; And be warming up to 45 ~ 60 DEG C, stir 30 minutes;
Wherein, monomer can be a kind of, also can be two or more monomers;
4) taking reductive agent by 1 ‰ of amount of starch is dissolved in a small amount of deionized water;
5) remaining monomer and reductive agent are added dropwise to 3 simultaneously) shown in starch liquid in, time for adding 1 ~ 3 hour, controls the temperature of reaction liquid and is no more than 65 DEG C;
6) rear continuation stirring 10 minutes are dropwised;
7) taking terminator by 2 ~ 4 ‰ of amount of starch is dissolved in a small amount of deionized water, disposablely join in reactant, stir 10 ~ 20 minutes termination reactions, and add in NaOH solution and about adjusting pH value to 5, obtain paste, thickness liquid, be degradable sizing agent.
Starch described in step 1) is any one in W-Gum, wheat starch, sorghum starch, Starch rice, yam starch, tapioca (flour), pueraria starch, sweet potato starch etc.
Described irradiation field is any one in gamma-rays, X-ray, electron beam etc.
Reductive agent described in step 4) can be sulphite, as sodium bisulfite, and sulphite hydrogen ammonium etc.; Can also be sodium sulphite, potassiumiodide etc.
Natural organic high-molecular sizing agent of the present invention is applicable to the neighborhoods such as packaging, printing, construction work, textile printing and dyeing, shoemaking, biological medicine.
Beneficial effect of the present invention: 1) utilize radiation method to carry out physically modified to natural polymer, the method has that technique is simple, investment goods is few, cost is lower, final obtained sizing agent can biochemical quantity high, be easy to biological degradation, secondary pollution can not be caused to environment.
Embodiment
Below in conjunction with specific embodiment, set forth the present invention further, should be understood that these examples are only not used in for illustration of the present invention and limit the scope of the invention.In addition should be understood that after the content of having read the present invention's instruction, those skilled in the art can do work to the present invention and change or amendment, and these equivalent form of values fall within the application's appended claims limited range equally.
Embodiment 1:
A synthetic method for degradable sizing agent, comprises the following steps:
1) starch (W-Gum, viscosity 46mps, water ratio 13.14wt%) is placed in γ-
60in Co irradiation field, under aerobic conditions (as under air conditions) carry out irradiation, irradiation dose is 10kGy, and it is degraded, and obtains the pre-irradiation starch containing superoxide;
2) by the acid solution combination treatment 10 ~ 60 minutes of above-mentioned the starch ratio of 1:10 and 0.1mol/L in mass ratio;
3) measure the monomer containing vinyl or allylic by 50% of pre-irradiation starch quality, get wherein a part and above-mentioned starch liquid mixing; And be warming up to 45 ~ 60 DEG C, stir 30 minutes;
Wherein, monomer can be a kind of, also can be two or more monomers;
4) taking reductive agent by 1 ‰ of amount of starch is dissolved in a small amount of deionized water;
5) remaining monomer and reductive agent are added dropwise to 3 simultaneously) shown in starch liquid in, time for adding 1 ~ 3 hour, controls the temperature of reaction liquid and is no more than 65 DEG C;
6) rear continuation stirring 10 minutes are dropwised;
7) taking terminator by 2 ‰ of amount of starch is dissolved in a small amount of deionized water, disposablely join in reactant, stir 10 ~ 20 minutes termination reactions, and add about NaOH solution is neutralized to pH value to 5, obtain paste, thickness liquid, be degradable sizing agent.
The starch adhesive of gained all has good gluing effect to paper product, plastics, woodwork etc., and separately adopt aerobic respiration parametric method to carry out biodegradability evaluation to sizing agent, result shows, its five days chemical oxygen demand (COD) (BOD
5) be 0.47 with the ratio of biochemical oxygen demand (BOD) (CODCr), there is good biodegradability energy.
Embodiment 2:
A synthetic method for degradable sizing agent, comprises the following steps:
1) starch (W-Gum, viscosity 46mps, water ratio 13.14wt%) is placed in electron beam irradiation field, under aerobic conditions (as under air conditions) carry out irradiation, irradiation dose is 20kGy, and it is degraded, and obtains the pre-irradiation starch containing superoxide;
2) by the acid solution combination treatment 10 ~ 60 minutes of above-mentioned the starch ratio of 1:10 and 0.1mol/L in mass ratio;
3) measure the monomer containing vinyl or allylic by 70% of pre-irradiation starch quality, get wherein a part and above-mentioned starch liquid mixing; And be warming up to 45 ~ 60 DEG C, stir 30 minutes;
Wherein, monomer can be a kind of, also can be two or more monomers;
4) taking reductive agent by 1 ‰ of amount of starch is dissolved in a small amount of deionized water;
5) remaining monomer and reductive agent are added dropwise to 3 simultaneously) shown in starch liquid in, time for adding 1 ~ 3 hour, controls the temperature of reaction liquid and is no more than 65 DEG C;
6) rear continuation stirring 10 minutes are dropwised;
7) taking terminator by 2 ‰ of amount of starch is dissolved in a small amount of deionized water, disposablely join in reactant, stir 10 ~ 20 minutes termination reactions, and add about NaOH solution is neutralized to pH value to 5, obtain paste, thickness liquid, be degradable sizing agent.
The starch adhesive of gained all has good gluing effect to paper product, plastics, woodwork etc., and separately adopt aerobic respiration parametric method to carry out biodegradability evaluation to sizing agent, result shows, its five days chemical oxygen demand (COD) (BOD
5) be 0.45 with the ratio of biochemical oxygen demand (BOD) (CODCr), there is good biodegradability energy.
Embodiment 3:
A synthetic method for degradable sizing agent, comprises the following steps:
1) starch (wheat starch, viscosity 42mps, water ratio 14.09wt%) is placed in γ-
60in Co irradiation field, under aerobic conditions (as under air conditions) carry out irradiation, irradiation dose is 30kGy, and it is degraded, and obtains the pre-irradiation starch containing superoxide;
2) by the acid solution combination treatment 10 ~ 60 minutes of above-mentioned the starch ratio of 1:10 and 0.1mol/L in mass ratio;
3) measure the monomer containing vinyl or allylic by 80% of pre-irradiation starch quality, get wherein a part and above-mentioned starch liquid mixing; And be warming up to 45 ~ 60 DEG C, stir 30 minutes;
Wherein, monomer can be a kind of, also can be two or more monomers;
4) taking reductive agent by 1 ‰ of amount of starch is dissolved in a small amount of deionized water;
5) remaining monomer and reductive agent are added dropwise to 3 simultaneously) shown in starch liquid in, time for adding 1 ~ 3 hour, controls the temperature of reaction liquid and is no more than 65 DEG C;
6) rear continuation stirring 10 minutes are dropwised;
7) taking terminator by 4 ‰ of amount of starch is dissolved in a small amount of deionized water, disposablely join in reactant, stir 10 ~ 20 minutes termination reactions, and add about NaOH solution is neutralized to pH value to 5, obtain paste, thickness liquid, be degradable sizing agent.
The starch adhesive of gained all has good gluing effect to paper product, plastics, woodwork etc., and separately adopt aerobic respiration parametric method to carry out biodegradability evaluation to sizing agent, result shows, its five days chemical oxygen demand (COD) (BOD
5) be 0.42 with the ratio of biochemical oxygen demand (BOD) (CODCr), there is good biodegradability energy.
Embodiment 4:
A synthetic method for degradable sizing agent, comprises the following steps:
1) starch (yam starch, viscosity 49mps, water ratio 13.51wt%) is placed in γ-
60in Co irradiation field, under aerobic conditions (as under air conditions) carry out irradiation, irradiation dose is 50kGy, and it is degraded, and obtains the pre-irradiation starch containing superoxide;
2) by the acid solution combination treatment 10 ~ 60 minutes of above-mentioned the starch ratio of 1:10 and 0.1mol/L in mass ratio;
3) measure the monomer containing vinyl or allylic by 100% of pre-irradiation starch quality, get wherein a part and above-mentioned starch liquid mixing; And be warming up to 45 ~ 60 DEG C, stir 30 minutes;
Wherein, monomer can be a kind of, also can be two or more monomers;
4) taking reductive agent by 1 ‰ of amount of starch is dissolved in a small amount of deionized water;
5) remaining monomer and reductive agent are added dropwise to 3 simultaneously) shown in starch liquid in, time for adding 1 ~ 3 hour, controls the temperature of reaction liquid and is no more than 65 DEG C;
6) rear continuation stirring 10 minutes are dropwised;
7) taking terminator by 2 ‰ of amount of starch is dissolved in a small amount of deionized water, disposablely join in reactant, stir 10 ~ 20 minutes termination reactions, and add about NaOH solution is neutralized to pH value to 5, obtain paste, thickness liquid, be degradable sizing agent.
The starch adhesive of gained all has good gluing effect to paper product, plastics, woodwork etc., separately aerobic respiration parametric method is adopted to carry out biodegradability evaluation to sizing agent, result shows, the ratio of its five days chemical oxygen demand (COD) (BOD5) and biochemical oxygen demand (BOD) (CODCr) is 0.44, has good biodegradability energy.
Embodiment 5:
A synthetic method for degradable sizing agent, comprises the following steps:
1) starch (yam starch, viscosity 49mps, water ratio 13.51wt%) is placed in electron beam irradiation field, under aerobic conditions (as under air conditions) carry out irradiation, irradiation dose is 20kGy, and it is degraded, and obtains the pre-irradiation starch containing superoxide;
2) by the acid solution combination treatment 10 ~ 60 minutes of above-mentioned the starch ratio of 1:10 and 0.1mol/L in mass ratio;
3) measure the monomer containing vinyl or allylic by 120% of pre-irradiation starch quality, get wherein a part and above-mentioned starch liquid mixing; And be warming up to 45 ~ 60 DEG C, stir 30 minutes;
Wherein, monomer can be a kind of, also can be two or more monomers;
4) taking reductive agent by 1 ‰ of amount of starch is dissolved in a small amount of deionized water;
5) remaining monomer and reductive agent are added dropwise to 3 simultaneously) shown in starch liquid in, time for adding 1 ~ 3 hour, controls the temperature of reaction liquid and is no more than 65 DEG C;
6) rear continuation stirring 10 minutes are dropwised;
7) taking terminator by 4 ‰ of amount of starch is dissolved in a small amount of deionized water, disposablely join in reactant, stir 10 ~ 20 minutes termination reactions, and add about NaOH solution is neutralized to pH value to 5, obtain paste, thickness liquid, be degradable sizing agent.
The starch adhesive of gained all has good gluing effect to paper product, plastics, woodwork etc., and separately adopt aerobic respiration parametric method to carry out biodegradability evaluation to sizing agent, result shows, its five days chemical oxygen demand (COD) (BOD
5) be 0.45 with the ratio of biochemical oxygen demand (BOD) (CODCr), there is good biodegradability energy.
Other kind of kind of starch also realizes by the present invention, does not operate one by one at this.Each raw material cited by the present invention and the bound value of each raw material, and the bound value of each processing parameter, can realize the present invention, not enumerate embodiment at this.
Claims (3)
1. a synthetic method for degradable sizing agent, is characterized in that comprising the following steps:
1) starch is placed in irradiation field, under aerobic conditions, carries out irradiation, irradiation dose 2 ~ 100kGy, make it degrade, obtain the pre-irradiation starch containing superoxide;
2) by the acid solution combination treatment 10 ~ 60 minutes of above-mentioned the starch ratio of 1:10 and 0.1mol/L in mass ratio;
3) measure the monomer containing vinyl or allylic by 50% ~ 200% of pre-irradiation starch quality, get wherein a part and above-mentioned starch liquid mixing; And be warming up to 45 ~ 60 DEG C, stir 30 minutes;
Wherein, monomer can be a kind of, also can be two or more monomers;
4) taking reductive agent by 1 ‰ of amount of starch is dissolved in a small amount of deionized water;
5) remaining monomer and reductive agent are added dropwise to 3 simultaneously) shown in starch liquid in, time for adding 1 ~ 3 hour, controls the temperature of reaction liquid and is no more than 65 DEG C;
6) rear continuation stirring 10 minutes are dropwised;
7) taking terminator by 2 ~ 4 ‰ of amount of starch is dissolved in a small amount of deionized water, disposablely join in reactant, stir 10 ~ 20 minutes termination reactions, and add about NaOH solution is neutralized to pH value to 5, obtain paste, thickness liquid, be degradable sizing agent.
2. the synthetic method of a kind of degradable sizing agent according to claim 1, is characterized in that: the starch described in step 1) is any one in W-Gum, wheat starch, sorghum starch, Starch rice, yam starch, tapioca (flour), pueraria starch, sweet potato starch; Described irradiation field is any one in gamma-rays, X-ray, electron beam etc.; Esters of acrylic acid described in step 3) is any one in methyl acrylate, ethyl propenoate, butyl acrylate, methyl methacrylate, butyl methacrylate, MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride, acrylyl oxy-ethyl-trimethyl salmiac etc.; Described reductive agent can be ceric ammonium nitrate, the redox system that Potassium Persulphate and S-WAT or ammonium persulphate and S-WAT form.
3. the synthetic method of a kind of degradable sizing agent according to claim 1, is characterized in that reaction is carried out under encloses container: react 2 ~ 3 hours under 50 DEG C ~ 55 DEG C conditions.
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| CN106381104A (en) * | 2016-10-20 | 2017-02-08 | 北京林业大学 | Water-based adhesive and preparation method thereof |
| CN107286867A (en) * | 2017-06-21 | 2017-10-24 | 合肥龙发包装有限公司 | A kind of preparation technology of corrugated case high-quality adhesive |
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Application publication date: 20150729 |