CN111087944A - Composite modified starch adhesive and preparation method thereof - Google Patents
Composite modified starch adhesive and preparation method thereof Download PDFInfo
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- CN111087944A CN111087944A CN201811245002.1A CN201811245002A CN111087944A CN 111087944 A CN111087944 A CN 111087944A CN 201811245002 A CN201811245002 A CN 201811245002A CN 111087944 A CN111087944 A CN 111087944A
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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
- C09J103/00—Adhesives based on starch, amylose or amylopectin or on their derivatives or degradation products
- C09J103/04—Starch derivatives
- C09J103/10—Oxidised starch
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B30/00—Preparation of starch, degraded or non-chemically modified starch, amylose, or amylopectin
- C08B30/04—Extraction or purification
- C08B30/042—Extraction or purification from cereals or grains
- C08B30/044—Extraction or purification from cereals or grains from corn or maize
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B30/00—Preparation of starch, degraded or non-chemically modified starch, amylose, or amylopectin
- C08B30/04—Extraction or purification
- C08B30/042—Extraction or purification from cereals or grains
- C08B30/046—Extraction or purification from cereals or grains from wheat
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B31/00—Preparation of derivatives of starch
- C08B31/003—Crosslinking of starch
- C08B31/006—Crosslinking of derivatives of starch
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B31/00—Preparation of derivatives of starch
- C08B31/18—Oxidised starch
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
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- 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
- C09J11/06—Non-macromolecular additives organic
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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
- C09J11/08—Macromolecular additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/38—Boron-containing compounds
- C08K2003/387—Borates
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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- 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)
- Inorganic Chemistry (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention relates to a composite modified starch adhesive and a preparation method thereof, and the composite modified adhesive comprises the following raw materials in parts by weight: 50-60 parts of corn starch, 30-40 parts of wheat starch, 3-8 parts of sodium hypochlorite, 1-5 parts of a reducing agent, 10-15 parts of 10% sodium hydroxide, 5-10 parts of hexamethoxymethyl melamine, 30-50 parts of polyvinyl alcohol, 1-5 parts of citric acid, 1-2 parts of melamine formaldehyde resin, 10-15 parts of an emulsifier, 1-3 parts of borax, 1-2 parts of an antifoaming agent, 5-10 parts of light calcium carbonate and 150 parts of deionized water. According to the composite modified starch adhesive, the hydroxyl groups in the starch molecules are oxidized, crosslinked and polymerized, and the melamine formaldehyde resin is used for modification and crosslinking, so that the water resistance of the adhesive is obviously improved, and the viscosity of the adhesive is greatly improved.
Description
Technical Field
The invention relates to the technical field of adhesive production, in particular to a composite modified starch adhesive and a preparation method thereof.
Technical Field
The adhesive is a technology for connecting the surfaces of homogeneous or heterogeneous objects together by using the adhesive, and has the characteristics of continuous stress distribution, light weight, low process temperature and the like. The glue joint is particularly suitable for connecting different materials, different thicknesses, ultrathin specifications and complex components. The adhesive joint is the fastest in recent development and has wide application industry. The amount of the wood industrial adhesive in China accounts for 80% of the total amount of the national adhesive, and the adhesive used by the artificial board is synthetic polymer or natural polymer.
Starch is a natural polymer material produced by plant photosynthesis, has wide sources, has gelling property and thickening property, and can form a film. However, the bonding property of starch does not reach the strength required by artificial boards, and the application of starch is seriously hindered. The hydroxyl in the starch molecule has high activity and is easy to react, and the starch can be chemically modified through the hydroxyl. It has been found that various properties of modified starch can be improved after modification by oxidation, etherification, grafting and crosslinking, but further research on viscosity and water resistance of the modified starch is needed.
Disclosure of Invention
Based on the above, the invention aims to provide a composite modified starch adhesive to effectively overcome the defects in the prior art.
In order to achieve the purpose, the invention adopts the following technical scheme:
the composite modified starch adhesive comprises the following raw materials in parts by weight: 50-60 parts of corn starch, 30-40 parts of wheat starch, 3-8 parts of sodium hypochlorite, 1-5 parts of a reducing agent, 10-15 parts of 10% sodium hydroxide, 5-10 parts of hexamethoxymethyl melamine, 30-50 parts of polyvinyl alcohol, 1-5 parts of citric acid, 1-2 parts of melamine formaldehyde resin, 10-15 parts of an emulsifier, 1-3 parts of borax, 1-2 parts of an antifoaming agent, 5-10 parts of light calcium carbonate and 150 parts of deionized water.
Compared with the prior art, the modified starch adhesive disclosed by the invention has the advantages that the viscosity and the water resistance of the adhesive are obviously improved by oxidizing, crosslinking and polymerizing hydroxyl groups in starch molecules and carrying out modified crosslinking by using melamine formaldehyde resin.
Further, the reducing agent is sodium sulfite.
Further, the defoaming agent is silicone oil or caprylic acid.
Further, the emulsifier is sodium dodecyl benzene sulfonate.
The invention also provides a preparation method of the composite modified starch adhesive, which comprises the following steps:
(1) and (3) pretreating the crude starch: adding the corn starch and the wheat starch in parts by weight into a dilute alkali solution with the pH value of 8-9, soaking and stirring for 40-60 minutes, then sieving with a 100-mesh sieve, standing and precipitating the starch milk, filtering and discharging wastewater to obtain the treated starch;
(2) and oxidizing: adding a proper amount of deionized water into the starch obtained in the step (1), heating to 55-60 ℃, and rapidly stirring for dissolving to obtain a starch solution; sequentially adding sodium hypochlorite into the starch solution, continuously heating to 85-90 ℃, stirring for reacting for 50-70 minutes, adding sodium sulfite serving as a reducing agent, and cooling to room temperature to obtain an oxidized starch solution;
(3) and pasting: adding hot sodium hydroxide with the mass fraction of 10% into the oxidized starch solution obtained in the step (2), uniformly stirring, adding a defoaming agent, and continuously stirring for 30-40 minutes to complete gelatinization to obtain starch paste;
(4) and (3) crosslinking polymerization: adding hexamethoxy methyl melamine and polyvinyl alcohol into the starch paste obtained in the step (3) under stirring, heating to 70-80 ℃, stirring for 5 minutes, adding citric acid, keeping the temperature unchanged, carrying out crosslinking reaction for 60-80 minutes, and cooling the reaction liquid to 50-55 ℃ after the reaction is finished; obtaining cross-linked starch;
(5) modification of melamine formaldehyde resin: adding melamine formaldehyde resin into the cross-linked starch obtained in the step (4), adding an emulsifier at the same time, adjusting the pH value of the solution to 9-10, keeping the temperature of 50-55 ℃ unchanged, and reacting for 3-4 hours to obtain composite modified starch paste;
(6) and (3) subsequent treatment: and (3) adding borax into the modified starch paste obtained in the step (5) for complexing, keeping the temperature unchanged, adding a proper amount of deionized water, stirring for 5-10 minutes, adding light calcium carbonate, stirring for 10-15 minutes, and cooling to room temperature to obtain the composite modified starch adhesive.
Compared with the prior art, the preparation method of the composite modified starch adhesive has the advantages that the starch is pretreated to reduce protein components in the starch, the protein is prevented from being coagulated with borax added in the later period, then, a proper oxidant and a proper reducing agent are selected for pre-oxidation, then, hexamethoxy methyl melamine is used as a cross-linking agent, citric acid is used as a catalyst for polymerization and cross-linking reaction, after the reaction, the starch molecules are cross-linked again through melamine formaldehyde resin, and the adhesive with high viscosity and good water resistance is obtained through a series of modification.
Further, the dilute alkali solution used in the step (1) is an ammonia water solution with the mass fraction of 3%, and the weight ratio of the dilute alkali solution to the starch is 1.5-1: 1.
For a better understanding and practice, the present invention is described in detail below.
Detailed Description
The technical solution of the present invention will be described in detail with reference to specific embodiments. The following examples are only for illustrating the technical solutions of the present invention more clearly, and therefore are only examples, and the protection scope of the present invention is not limited thereby.
The invention provides a composite modified starch adhesive which comprises the following raw materials in parts by weight: 50-60 parts of corn starch, 30-40 parts of wheat starch, 3-8 parts of sodium hypochlorite, 1-5 parts of a reducing agent, 10-15 parts of 10% sodium hydroxide, 5-10 parts of hexamethoxymethyl melamine, 30-50 parts of polyvinyl alcohol, 1-5 parts of citric acid, 1-2 parts of melamine formaldehyde resin, 10-15 parts of an emulsifier, 1-3 parts of borax, 1-2 parts of an antifoaming agent, 5-10 parts of light calcium carbonate and 150 parts of deionized water.
Preferably, the reducing agent is sodium sulfite.
Preferably, the defoaming agent is silicone oil or caprylic acid.
Preferably, the emulsifier is sodium dodecyl benzene sulfonate.
The preparation method is illustrated by specific examples
Table 1 shows the ingredients and the corresponding parts by weight of examples 1-3
The preparation method of the composite modified starch adhesive of the embodiments 1 to 3 comprises the following steps:
(1) and (3) pretreating the crude starch: adding the corn starch and the wheat starch in parts by weight into a dilute alkali solution with the pH value of 8-9, soaking and stirring for 40-60 minutes, then sieving with a 100-mesh sieve, standing and precipitating the starch milk, filtering and discharging wastewater to obtain the treated starch;
(2) and oxidizing: adding a proper amount of deionized water into the starch obtained in the step (1), heating to 55-60 ℃, and rapidly stirring for dissolving to obtain a starch solution; sequentially adding sodium hypochlorite into the starch solution, continuously heating to 85-90 ℃, stirring for reacting for 50-70 minutes, adding sodium sulfite serving as a reducing agent, and cooling to room temperature to obtain an oxidized starch solution;
(3) and pasting: adding hot sodium hydroxide with the mass fraction of 10% into the oxidized starch solution obtained in the step (2), uniformly stirring, adding a defoaming agent, and continuously stirring for 30-40 minutes to complete gelatinization to obtain starch paste;
(4) and (3) crosslinking polymerization: adding hexamethoxy methyl melamine and polyvinyl alcohol into the starch paste obtained in the step (3) under stirring, heating to 70-80 ℃, stirring for 5 minutes, adding citric acid, keeping the temperature unchanged, carrying out crosslinking reaction for 60-80 minutes, and cooling the reaction liquid to 50-55 ℃ after the reaction is finished; obtaining cross-linked starch;
(5) modification of melamine formaldehyde resin: adding melamine formaldehyde resin into the cross-linked starch obtained in the step (4), adding an emulsifier at the same time, adjusting the pH value of the solution to 9-10, keeping the temperature of 50-55 ℃ unchanged, and reacting for 3-4 hours to obtain composite modified starch paste;
(6) and (3) subsequent treatment: and (3) adding borax into the modified starch paste obtained in the step (5) for complexing, keeping the temperature unchanged, adding a proper amount of deionized water, stirring for 5-10 minutes, adding light calcium carbonate, stirring for 10-15 minutes, and cooling to room temperature to obtain the composite modified starch adhesive.
The diluted alkaline solution used in the step (1) is a diluted ammonia water solution with the mass fraction of 3%, and the weight ratio of the diluted alkaline solution to the starch is 1.5-1: 1.
The control example was an oxidatively modified starch adhesive, i.e. the control example did not perform step (4) and step (5), but only steps (1), (2), (3) and (6).
Water resistance time test Water resistance was tested according to QB/T1094-1991: the sample was adhered and cured for 3d, and immersed in normal temperature water and 80 ℃ hot water, respectively. The former is soaked for 30 days, the latter is soaked for 15 days, and whether the glue is broken or not is observed and recorded.
And (3) viscosity testing: the viscosity measurement was carried out with a digital viscometer according to the standard of GB/T2794-1995.
Table 2 shows the results of the tests carried out on examples 1 to 3 in comparison with the control examples;
from the above table, it is clear that the adhesive of the present invention has good water resistance and higher viscosity than the comparative examples.
The above description is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, it is possible to make various changes and modifications without departing from the structure of the present invention, and it should be considered as the protection scope of the present invention, which will not affect the effect of the implementation of the present invention and the practicability of the patent.
Claims (6)
1. The composite modified starch adhesive is characterized by comprising the following raw materials in parts by weight: 50-60 parts of corn starch, 30-40 parts of wheat starch, 3-8 parts of sodium hypochlorite, 1-5 parts of a reducing agent, 10-15 parts of 10% sodium hydroxide, 5-10 parts of hexamethoxymethyl melamine, 30-50 parts of polyvinyl alcohol, 1-5 parts of citric acid, 1-2 parts of melamine formaldehyde resin, 10-15 parts of an emulsifier, 1-3 parts of borax, 1-2 parts of an antifoaming agent, 5-10 parts of light calcium carbonate and 150 parts of deionized water.
2. The composite modified starch adhesive as claimed in claim 1, wherein the reducing agent is sodium sulfite.
3. The composite modified starch adhesive of claim 2, wherein the defoaming agent is silicone oil or caprylic acid.
4. The composite modified starch adhesive of claim 3, wherein the emulsifier is sodium dodecylbenzene sulfonate.
5. A method for preparing the composite modified starch adhesive as claimed in claim 4, which comprises the following steps:
(1) and (3) pretreating the crude starch: adding the corn starch and the wheat starch in parts by weight into a dilute alkali solution with the pH value of 8-9, soaking and stirring for 40-60 minutes, then sieving with a 100-mesh sieve, standing and precipitating the starch milk, filtering and discharging wastewater to obtain the treated starch;
(2) and oxidizing: adding a proper amount of deionized water into the starch obtained in the step (1), heating to 55-60 ℃, and rapidly stirring for dissolving to obtain a starch solution; sequentially adding sodium hypochlorite into the starch solution, continuously heating to 85-90 ℃, stirring for reacting for 50-70 minutes, adding sodium sulfite serving as a reducing agent, and cooling to room temperature to obtain an oxidized starch solution;
(3) and pasting: adding hot sodium hydroxide with the mass fraction of 10% into the oxidized starch solution obtained in the step (2), uniformly stirring, adding a defoaming agent, and continuously stirring for 30-40 minutes to complete gelatinization to obtain starch paste;
(4) and (3) crosslinking polymerization: adding hexamethoxy methyl melamine and polyvinyl alcohol into the starch paste obtained in the step (3) under stirring, heating to 70-80 ℃, stirring for 5 minutes, adding citric acid, keeping the temperature unchanged, carrying out crosslinking reaction for 60-80 minutes, and cooling the reaction liquid to 50-55 ℃ after the reaction is finished; obtaining cross-linked starch;
(5) modification of melamine formaldehyde resin: adding melamine formaldehyde resin into the cross-linked starch obtained in the step (4), adding an emulsifier at the same time, adjusting the pH value of the solution to 9-10, keeping the temperature of 50-55 ℃ unchanged, and reacting for 3-4 hours to obtain composite modified starch paste;
(6) and (3) subsequent treatment: and (3) adding borax into the modified starch paste obtained in the step (5) for complexing, keeping the temperature unchanged, adding a proper amount of deionized water, stirring for 5-10 minutes, adding light calcium carbonate, stirring for 10-15 minutes, and cooling to room temperature to obtain the composite modified starch adhesive.
6. The preparation method of the composite modified starch adhesive as claimed in claim 5, wherein the dilute alkali solution used in the step (1) is a dilute ammonia solution with a mass fraction of 3%, and the weight ratio of the dilute alkali solution to the starch is 1.5-1: 1.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811245002.1A CN111087944A (en) | 2018-10-24 | 2018-10-24 | Composite modified starch adhesive and preparation method thereof |
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| CN201811245002.1A CN111087944A (en) | 2018-10-24 | 2018-10-24 | Composite modified starch adhesive and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115678574A (en) * | 2022-10-24 | 2023-02-03 | 北京建筑材料科学研究总院有限公司 | Single-component intumescent flame retardant and preparation method and application thereof |
| CN117887383A (en) * | 2024-03-18 | 2024-04-16 | 潍坊市农业科学院(山东省农业科学院潍坊市分院) | Preparation method and application of plant fixing adhesive |
-
2018
- 2018-10-24 CN CN201811245002.1A patent/CN111087944A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115678574A (en) * | 2022-10-24 | 2023-02-03 | 北京建筑材料科学研究总院有限公司 | Single-component intumescent flame retardant and preparation method and application thereof |
| CN117887383A (en) * | 2024-03-18 | 2024-04-16 | 潍坊市农业科学院(山东省农业科学院潍坊市分院) | Preparation method and application of plant fixing adhesive |
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Application publication date: 20200501 |