CN110903407A - Oxidized starch and preparation method thereof - Google Patents

Oxidized starch and preparation method thereof Download PDF

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Publication number
CN110903407A
CN110903407A CN201911332569.7A CN201911332569A CN110903407A CN 110903407 A CN110903407 A CN 110903407A CN 201911332569 A CN201911332569 A CN 201911332569A CN 110903407 A CN110903407 A CN 110903407A
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oxidized starch
parts
reaction
starch
reaction kettle
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CN201911332569.7A
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缪鹏飞
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Nantong Tongdi Biotechnology Co Ltd
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Nantong Tongdi Biotechnology Co Ltd
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Priority to CN201911332569.7A priority Critical patent/CN110903407A/en
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08BPOLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B31/00Preparation of derivatives of starch
    • C08B31/18Oxidised starch

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

Abstract

The invention discloses oxidized starch, which comprises the following components in percentage by mass: 3500 parts of corn starch; 55-65 parts of oxidant with the hydrogen ion concentration of 30%; 57-62 parts of a terminator; 1-1.5 parts of a reducing agent. The preparation process of the oxidized starch directly uses the corn starch without adding water for production, liquid or gas with high acid concentration can not be generated, and the environment can not be polluted.

Description

Oxidized starch and preparation method thereof
Technical Field
The invention relates to the field of modified starch preparation, in particular to oxidized starch and a preparation method thereof.
Background
With the continuous development of current social economy, the demand of people for environment-friendly materials is continuously improved, and the development of adhesive materials which are environment-friendly, low in price and excellent in performance becomes the main target of research of people at present.
The starch adhesive has become an ideal substitute product for the traditional synthetic resin adhesive due to the characteristics of wide raw material sources, low price, nature, no stimulation, simple production process and the like. However, due to the self-structure of the starch adhesive, the problems of poor water resistance, low solid content, short pot life and the like become short boards which restrict the development of the starch adhesive. Therefore, modification research needs to be carried out on the starch adhesive, common modification methods comprise physical modification, chemical modification, biological modification and the like, and the starch adhesive with different properties developed through the chemical modification is widely applied. The chemical modification is a method for changing the physical and chemical properties of starch by adopting different chemical reagents to carry out chemical reaction with the starch, and is also a starch modification method which is most widely applied. The most common chemical modification in industrial production is oxidative modification.
The existing oxidation preparation method can generate a large amount of liquid with higher acid concentration in the preparation process, can cause environmental pollution when discharged into the environment, has higher preparation cost, and is not beneficial to industrialized mass production.
Therefore, the development of an energy-saving and environment-friendly preparation method is a technical problem which needs to be solved urgently by the technical personnel in the field.
Disclosure of Invention
In order to solve the technical problems, the invention aims to provide oxidized starch and a preparation method thereof, wherein acid liquid is not generated in the preparation process of the oxidized starch, so that the oxidized starch is energy-saving and environment-friendly and can avoid pollution.
The application provides oxidized starch which comprises the following components in percentage by mass: 3500 parts of corn starch; 55-65 parts of oxidant with the hydrogen ion concentration of 30%; 57-62 parts of a terminator; 1-1.5 parts of a reducing agent.
Optionally, the oxidant comprises acid and a composite oxidant, and specifically comprises 55-65 parts of 30% hydrogen peroxide, 1.5-2.5 parts of ammonium peroxide and 1.5-2.5 parts of potassium persulfate.
Optionally, the terminating agent is sodium carbonate; the reducing agent is sodium thiosulfate.
Optionally, the corn starch adhesive further comprises a tackifier, wherein the tackifier comprises polyacrylamide and resin, the mass of the polyacrylamide is 0.09-0.12% of that of the corn starch, and the mass of the resin is 0.35-0.41% of that of the corn starch.
Optionally, 3500 kg of corn starch, 57 kg of 30% hydrogen peroxide, 2 kg of ammonium peroxide, 2 kg of potassium persulfate, 60 kg of sodium carbonate, 1 kg of sodium thiosulfate, 3.5 kg of polyacrylamide and 14 kg of resin are included.
The application also provides a preparation method of the oxidized starch, which is used for preparing the oxidized starch of any one of the above items, and comprises the following steps: s1: heating a reaction kettle to 50 ℃, then putting corn starch into the reaction kettle, starting a stirring blade in the reaction kettle, and setting the rotating speed of the stirring blade to be 60-100 r/min; s2: putting ammonium peroxide and potassium persulfate into the reaction kettle, starting to spray hydrogen peroxide, starting timing after spraying is finished, wherein the reaction time is 60-90 minutes, and the stirring blades keep rotating in the putting process and the reaction process; s3: simultaneously adding a reducing agent and a terminating agent into a reaction kettle, and stirring for a first preset time; s4: adding a tackifier, reacting for a second preset time, and simultaneously controlling the pH value to be 6.5-7.5;
s5: and after the reaction is finished, drying, crushing and sieving the powder to obtain the oxidized starch.
Optionally, the first predetermined time is 10 minutes and the second predetermined time is 20 minutes.
Optionally, 3500 kg of oxidized starch is put into the reaction kettle in step S1; step S2, adding 2 kg of ammonium peroxide, 2 kg of potassium persulfate and 57 kg of 30% hydrogen peroxide into the reaction kettle; step S3, adding 60 kg of sodium carbonate and 1 kg of sodium thiosulfate into the reaction kettle, and stirring for 10 minutes; in step S4, 3.5 kg of polyacrylamide and 14 kg of resin were charged into the reaction vessel and reacted for 20 minutes.
Compared with the prior art, the technical scheme of the invention has the following advantages:
the preparation process of the oxidized starch directly uses the corn starch without adding water for production, liquid or gas with high acid concentration can not be generated, and the environment can not be polluted.
Detailed Description
The present invention will be described in detail with reference to specific embodiments. It should be understood that the detailed description and specific examples, while indicating the present invention, are given by way of illustration and explanation only, not limitation.
In a specific embodiment, the invention provides oxidized starch, which comprises the following components in percentage by mass: 3500 parts of corn starch; 55-65 parts of oxidant with the hydrogen ion concentration of 30%; 57-62 parts of a terminator; 1-1.5 parts of a reducing agent.
The preparation process of the oxidized starch does not add water, the corn starch is directly used for production, liquid with high acid concentration can not be generated, and the environment can not be polluted.
Specifically, the oxidant comprises acid and a composite oxidant, and specifically comprises 55-65 parts of 30% hydrogen peroxide, 1.5-2.5 parts of ammonium peroxide and 1.5-2.5 parts of potassium persulfate. The terminating agent is sodium carbonate; the reducing agent is sodium thiosulfate.
The ammonium peroxide is a composite oxide, and in the reaction process, the composite oxide combines acidification and oxidation, so that the corn starch with different chain lengths participates in the reaction, the reaction of the corn starch is more thorough, and the composite oxide can also be potassium permanganate.
In a further embodiment, the corn starch adhesive further comprises a tackifier, wherein the tackifier comprises polyacrylamide and resin, the mass of the polyacrylamide is 0.09% -0.12% of the mass of the corn starch, and the mass of the resin is 0.35% -0.41% of the mass of the corn starch.
The viscosity of the glue prepared from the corn starch can be controlled by controlling the amount of acid and the reaction time, and a tackifier can be additionally added, and the production process can be adjusted according to the use requirement of the glue.
In a preferred embodiment, the mass ratio of each component of the oxidized starch is: 3500 kg of corn starch, 57 kg of 30% hydrogen peroxide, 2 kg of ammonium peroxide, 2 kg of potassium persulfate, 60 kg of sodium carbonate, 1 kg of sodium thiosulfate, 3.5 kg of polyacrylamide and 14 kg of resin.
The invention also provides a preparation method of oxidized starch, which is used for preparing the oxidized starch of each embodiment and comprises the following steps:
step S1: heating a reaction kettle to 50 ℃, then putting corn starch into the reaction kettle, starting a stirring blade in the reaction kettle, and setting the rotating speed of the stirring blade to be 60-100 r/min;
step S2: putting ammonium peroxide and potassium persulfate into the reaction kettle, starting to spray hydrogen peroxide, starting timing after spraying is finished, wherein the reaction time is 60-90 minutes, and the stirring blades keep rotating in the putting process and the reaction process;
step S3: simultaneously adding a reducing agent and a terminating agent into a reaction kettle, and stirring for a first preset time;
step S4: adding a tackifier, reacting for a second preset time, and simultaneously controlling the pH value to be 6.5-7.5;
step S5: and after the reaction is finished, drying, crushing and sieving the powder to obtain the oxidized starch.
In the preparation process, the rotating speed of the stirring blades in the reaction kettle is selected according to the stirring effect of the blades; the reaction time after spraying the hydrogen peroxide directly affects the viscosity of the glue made of the oxidized starch, and the amount of the hydrogen peroxide sprayed also affects the viscosity of the glue made of the oxidized starch. Specifically, in the reaction process, when the acid amount is large and the reaction time is long, the reaction is thorough, the molecules are fully oxidized, the molecular chain is short, and the viscosity of the glue is low.
Specifically, the first predetermined time may be about 10 minutes, and the second predetermined time may be about 20 minutes.
In a preferred embodiment, 3500 kg of corn starch is charged into the reaction vessel in step S1; step S2, adding 2 kg of ammonium peroxide, 2 kg of potassium persulfate and 57 kg of 30% hydrogen peroxide into the reaction kettle; step S3, adding 60 kg of sodium carbonate and 1 kg of sodium thiosulfate into the reaction kettle, and stirring for 10 minutes; in step S4, 3.5 kg of polyacrylamide and 14 kg of resin were charged into the reaction vessel and reacted for 20 minutes.
The first embodiment is as follows:
in the preparation process of the oxidized starch, a reaction kettle is heated to 50 ℃, 3500 kg of corn starch is put into the reaction kettle, a stirring blade in the reaction kettle is started, and the rotating speed of the stirring blade is set to be 100 r/min; 2.5 kg of ammonium peroxide and 2.5 kg of potassium persulfate are put into a reaction kettle, hydrogen peroxide is sprayed, the concentration of hydrogen ions is 30%, 65 kg of hydrogen peroxide is sprayed in total, timing is started after the spraying is finished, the reaction time is 90 minutes, and stirring blades are always kept rotating in the putting process and the reaction process; putting 62 kg of sodium carbonate and 1.5 kg of sodium thiosulfate into a reaction kettle, and stirring for 10 minutes; 2.88 kg of polyacrylamide and 11.2 kg of resin are added for reaction for 20 minutes, and the pH value is controlled to be 6.5-7.5; the powder is dried after the reaction is finished, the powder is crushed and sieved to obtain oxidized starch, in the reaction process of the oxidized starch, the added hydrogen peroxide is excessive, the reaction time is long, the reaction is thorough, the molecules are fully oxidized, the molecular chains are short, the added tackifier is less, and the viscosity of the glue prepared from the oxidized starch is low, so that the oxidized starch is suitable for: it is suitable for the production of spiral paper tube and pagoda paper tube.
Example two:
in the preparation process of the oxidized starch, a reaction kettle is heated to 50 ℃, 3500 kg of corn starch is put into the reaction kettle, a stirring blade in the reaction kettle is started, and the rotating speed of the stirring blade is set to be 80 r/min; 1.5 kg of ammonium peroxide and 1.5 kg of potassium persulfate are put into a reaction kettle, hydrogen peroxide is sprayed, the concentration of the hydrogen peroxide is 30 percent, 55 kg of hydrogen peroxide is sprayed in total, timing is started after the spraying is finished, the reaction time is 60 minutes, and stirring blades are always kept rotating in the putting process and the reaction process; putting 57 kg of sodium carbonate and 1 kg of sodium thiosulfate into a reaction kettle, and stirring for 10 minutes; 4.44 kg of polyacrylamide and 15.17 kg of resin are added for reaction for 20 minutes, and the pH value is controlled to be 6.5-7.5; the powder is dried, crushed and sieved after the reaction is finished to obtain oxidized starch, in the reaction process of the oxidized starch, less hydrogen peroxide is added, the reaction time is short, the molecular chain is long, more tackifier is added, and the viscosity of the glue prepared by using the oxidized starch is high, so that the oxidized starch is suitable for: the paper is suitable for paper products such as industrial paperboards and cartons.
The oxidized starch and the preparation method thereof provided by the present invention are described in detail above. The principles and embodiments of the present invention are explained herein using specific examples, which are presented only to assist in understanding the method and its core concepts. It should be noted that, for those skilled in the art, it is possible to make various improvements and modifications to the present invention without departing from the principle of the present invention, and those improvements and modifications also fall within the scope of the claims of the present invention.

Claims (8)

1. The oxidized starch is characterized by comprising the following components in percentage by mass: 3500 parts of corn starch; 55-65 parts of oxidant with the hydrogen ion concentration of 30%; 57-62 parts of a terminator; 1-1.5 parts of a reducing agent.
2. The oxidized starch according to claim 1, wherein the oxidizing agent comprises an acid and a composite oxidizing agent, and specifically comprises 55 to 65 parts of 30% hydrogen peroxide, 1.5 to 2.5 parts of ammonium peroxide, and 1.5 to 2.5 parts of potassium persulfate.
3. An oxidized starch according to claim 1, characterized in that the terminating agent is sodium carbonate; the reducing agent is sodium thiosulfate.
4. An oxidized starch according to claims 1 to 3 further comprising a tackifier, the tackifier comprising polyacrylamide and a resin, the polyacrylamide being present in an amount of 0.09 to 0.12% by mass and the resin being present in an amount of 0.35 to 0.41% by mass, based on the mass of the corn starch.
5. An oxidized starch according to claim 4 comprising 3500 kg of corn starch, 57 kg of 30% hydrogen peroxide, 2 kg of ammonium peroxide, 2 kg of potassium persulfate, 60 kg of sodium carbonate, 1 kg of sodium thiosulfate, 3.5 kg of polyacrylamide and 14 kg of resin.
6. A method for producing an oxidized starch according to any one of claims 1 to 5, comprising the steps of:
s1: heating a reaction kettle to 50 ℃, then putting corn starch into the reaction kettle, starting a stirring blade in the reaction kettle, and setting the rotating speed of the stirring blade to be 60-100 r/min;
s2: ammonium peroxide and potassium persulfate are put into the reaction kettle, and hydrogen peroxide starts to be sprayed in a manner that starch rolls down and acidic solution is sprayed upwards at the same time, so that the contact area of the starch and the oxidant is greatly increased. Timing is started after spraying is finished, the reaction time is 60-90 minutes, and the stirring blades keep rotating in the feeding process and the reaction process;
s3: simultaneously adding a reducing agent and a terminating agent into a reaction kettle, and stirring for a first preset time;
s4: adding a tackifier, reacting for a second preset time, and simultaneously controlling the pH value to be 6.5-7.5; s5: and after the reaction is finished, drying, crushing and sieving the powder to obtain the oxidized starch.
7. A method of producing oxidized starch according to claim 6, wherein the first predetermined time is 10 minutes and the second predetermined time is 20 minutes.
8. The method according to claim 7, wherein 3500 kg of oxidized starch is charged into the reaction vessel in step S1; step S2, adding 2 kg of ammonium peroxide, 2 kg of potassium persulfate and 57 kg of 30% hydrogen peroxide into the reaction kettle; step S3, adding 60 kg of sodium carbonate and 1 kg of sodium thiosulfate into the reaction kettle, and stirring for 10 minutes; in step S4, 3.5 kg of polyacrylamide and 14 kg of resin were charged into the reaction vessel and reacted for 20 minutes.
CN201911332569.7A 2019-12-22 2019-12-22 Oxidized starch and preparation method thereof Pending CN110903407A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102633891A (en) * 2012-04-19 2012-08-15 浙江益纸淀粉有限公司 AKD (alkyl ketene dimer) starch and preparation method thereof
CN106085289A (en) * 2016-07-26 2016-11-09 明辉大秦(上海)环保科技有限公司 Environment-friendly type corrugated board low temperature laminating starch adhesive and preparation method thereof
CN108659751A (en) * 2018-06-05 2018-10-16 佛山皖阳生物科技有限公司 A kind of preparation method of modified corn starch adhesive
CN108676223A (en) * 2018-04-19 2018-10-19 安徽华远节水灌溉器材有限公司 A kind of talc modified waste polyethylene
CN110128557A (en) * 2019-05-15 2019-08-16 河南汇泉生物科技有限公司 A kind of oxidized starch and preparation method thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102633891A (en) * 2012-04-19 2012-08-15 浙江益纸淀粉有限公司 AKD (alkyl ketene dimer) starch and preparation method thereof
CN106085289A (en) * 2016-07-26 2016-11-09 明辉大秦(上海)环保科技有限公司 Environment-friendly type corrugated board low temperature laminating starch adhesive and preparation method thereof
CN108676223A (en) * 2018-04-19 2018-10-19 安徽华远节水灌溉器材有限公司 A kind of talc modified waste polyethylene
CN108659751A (en) * 2018-06-05 2018-10-16 佛山皖阳生物科技有限公司 A kind of preparation method of modified corn starch adhesive
CN110128557A (en) * 2019-05-15 2019-08-16 河南汇泉生物科技有限公司 A kind of oxidized starch and preparation method thereof

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朱洪法 等: "《精细化工产品配方与制造》", 31 July 2001, 金盾出版社 *

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Application publication date: 20200324