CN109679044A - A kind of preparation method of the modified phenolic resin adhesive suitable for bond paper - Google Patents
A kind of preparation method of the modified phenolic resin adhesive suitable for bond paper Download PDFInfo
- Publication number
- CN109679044A CN109679044A CN201811574948.2A CN201811574948A CN109679044A CN 109679044 A CN109679044 A CN 109679044A CN 201811574948 A CN201811574948 A CN 201811574948A CN 109679044 A CN109679044 A CN 109679044A
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- Prior art keywords
- temperature
- phenolic resin
- preparation
- resin adhesive
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G8/00—Condensation polymers of aldehydes or ketones with phenols only
- C08G8/28—Chemically modified polycondensates
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G8/00—Condensation polymers of aldehydes or ketones with phenols only
- C08G8/04—Condensation polymers of aldehydes or ketones with phenols only of aldehydes
- C08G8/08—Condensation polymers of aldehydes or ketones with phenols only of aldehydes of formaldehyde, e.g. of formaldehyde formed in situ
- C08G8/10—Condensation polymers of aldehydes or ketones with phenols only of aldehydes of formaldehyde, e.g. of formaldehyde formed in situ with phenol
-
- 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
- C09J161/00—Adhesives based on condensation polymers of aldehydes or ketones; Adhesives based on derivatives of such polymers
- C09J161/04—Condensation polymers of aldehydes or ketones with phenols only
- C09J161/06—Condensation polymers of aldehydes or ketones with phenols only of aldehydes with phenols
- C09J161/14—Modified phenol-aldehyde condensates
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- General Chemical & Material Sciences (AREA)
- Phenolic Resins Or Amino Resins (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention discloses a kind of preparation methods of modified phenolic resin adhesive suitable for bond paper, phenol, catalyst are added in reaction kettle, within limits by temperature control, whole formaldehyde, which are added, makes it automatically continuously heat up, and bio-extract is added at a certain temperature, a period of time is finally reacted at 80~100 DEG C, when 4 glasss of viscosity of painting of reaction system reach 14~17s at 40 DEG C, just reaction was completed to get.Preparation method of the present invention starts to react in low temperature, easy to control；System heating is provided by raw material exothermic heat of reaction, can be heated up without heating and be saved the energy；And be modified using bio-extract, it can reduce environmental pollution.
Description
Technical field
The present invention relates to adhesive preparation field more particularly to a kind of modified phenolic resin adhesives suitable for bond paper
Preparation method.
Background technique
About 4,800,000 tons of world's phenolic resin yield in 2010, wherein phenolic resin adhesive accounts for about 33%.Phenolic resin because
Its unique cross-linked network molecular structure, has the advantages that bonding strength height, water-tolerant, good weatherability.But as petroleum provides
The worsening shortages and petroleum base chemical industry increasing price of raw materials in source, the large-scale production and application of wood-based plate phenolic resin adhesive
Increasingly it is restricted.
Bio-extract can partially substitute phenol and prepare modified phenolic resin adhesive, can both reduce cost, reach biology
The purpose of matter resources effective utilization, and the toxic remnants such as modified phenolic resin adhesive free phenol prepared are lower, have ring
Protect meaning.
Summary of the invention
The present invention is to solve the above problem in the prior art, proposes a kind of modified alkyd resin glue suitable for bond paper
The preparation method of glutinous agent.
To achieve the above object, the invention adopts the following technical scheme:
The first aspect of the invention is to provide a kind of preparation side of modified phenolic resin adhesive suitable for bond paper
Phenol, catalyst are added in reaction kettle method, and within limits by temperature control, whole formaldehyde, which are added, connects it automatically
Temperature of continuing rising, and bio-extract is added at a certain temperature, a period of time is finally reacted at 80~100 DEG C, to reaction system
4 glasss of viscosity of painting when reaching 14~17s at 40 DEG C, just reaction was completed to get.
Further, the preparation method of the modified phenolic resin adhesive suitable for bond paper, in parts by weight
Meter, each raw material dosage are as follows:
Further, the preparation method of the modified phenolic resin adhesive suitable for bond paper, in parts by weight
Meter, each raw material dosage are as follows:
Further, the preparation method of the modified phenolic resin adhesive suitable for bond paper, reaction system add
Temperature when entering the formaldehyde is 30~50 DEG C.
It is further preferred that the preparation method of the modified phenolic resin adhesive suitable for bond paper, reactant
The temperature when formaldehyde is added in system is 38~45 DEG C.
Further, the preparation method of the modified phenolic resin adhesive suitable for bond paper, reaction system add
Temperature when entering the bio-extract is 50~80 DEG C.
It is further preferred that the preparation method of the modified phenolic resin adhesive suitable for bond paper, reactant
The temperature when bio-extract is added in system is 60~75 DEG C.
Further, the preparation method of the modified phenolic resin adhesive suitable for bond paper, reaction system are anti-
Temperature at the end of answering is 80~100 DEG C.
Further, the preparation method of the modified phenolic resin adhesive suitable for bond paper, reaction system are anti-
Temperature at the end of answering is 85~95 DEG C.
Further, the preparation method of the modified phenolic resin adhesive suitable for bond paper, the catalyst
For one or more of barium hydroxide, calcium hydroxide, sodium hydroxide.
Further, the preparation method of the modified phenolic resin adhesive suitable for bond paper, the biology mention
It takes produce to be born in timber, is selected from one of paper waste corruption slurry, screenings, bark, medicament waste liquid, grass end, pulping waste liquor or several
Kind.
Further, the preparation method of the modified phenolic resin adhesive suitable for bond paper, the biology mention
It takes object not limit its existing forms, can be the liquid of solid or certain content.
Further, the preparation method of the modified phenolic resin adhesive suitable for bond paper, specifically include as
Lower step:
(1) reaction kettle is first added in phenol, catalyst, stirred；
(2) when temperature is controlled at 30~50 DEG C, formaldehyde is added, starts to control its temperature, makes its automatic heating；
(3) control reaction temperature is warming up to 50~80 DEG C, bio-extract and water is added, and continue to heat up；
(4) control reaction temperature is warming up to 80~100 DEG C, and after its temperature is stablized, it is viscous to detect its 4 glass of painting at 40 DEG C
Degree；
(5) when viscosity reaches 14~17s, start to cool down, reaction was completed, and detects viscosity when it is cooled to 40 DEG C.
The present invention by adopting the above technical scheme, compared with prior art, has the following technical effect that
(1) the method for the present invention starts to react in low temperature, easy to control；System heating is provided by raw material exothermic heat of reaction, without adding
Heat can heat up and save the energy；
(2) the small bond paper dipping that is more applicable for of the phenolic resin adhesive molecular weight produced using the present invention is used；
(3) present invention is modified using bio-extract, it is possible to reduce environmental pollution provides help to environmental protection.
Specific embodiment
The present invention is described in more detail below by specific embodiment, for a better understanding of the present invention,
But following embodiments are not intended to limit the scope of the invention.
Embodiment 1 is suitable for the preparation of the modified phenolic resin adhesive of bond paper
(1) by 10 parts of phenol, 0.1 part of sodium hydroxide is first added in reaction kettle, stirs 20min；
(2) when its temperature is stablized at 40 DEG C, 20 parts of formaldehyde are added, controller for water boiler temperature rises, and makes its automatic heating；
(3) when its temperature rises to 60 DEG C, 5 parts of bio-extracts and 10 parts of water are added, and continue to heat up；
(4) control reaction rises to 90 DEG C in 50min, and starts to keep the temperature at this temperature, and detects and glue for 4 glasss of painting at 40 DEG C
Degree；
(5) when its viscosity is in 14.5s or so, starting cooling discharge, reaction was completed, detects it when being finally cooled to 40 DEG C
Viscosity is 17s.
Embodiment 2 is suitable for the preparation of the modified phenolic resin adhesive of bond paper
(1) by 40 parts of phenol, 5 parts of sodium hydroxides are first added in reaction kettle, stir 20min；
(2) when its temperature is stablized at 40 DEG C, 100 parts of formaldehyde are added, controller for water boiler temperature rises, and rises it automatically
Temperature；
(3) when its temperature rises to 60 DEG C, 40 parts of bio-extracts and 30 parts of water are added, and continue to heat up；
(4) control reaction rises to 90 DEG C in 50min, and starts to keep the temperature at this temperature, and detects and glue for 4 glasss of painting at 40 DEG C
Degree；
(5) when its viscosity is in 14.8s or so, starting cooling discharge, reaction was completed, detects it when being finally cooled to 40 DEG C
Viscosity is 17.5s.
Embodiment 3 is suitable for the preparation of the modified phenolic resin adhesive of bond paper
(1) by 50 parts of phenol, 10 parts of sodium hydroxides are first added in reaction kettle, stir 20min；
(2) when its temperature is stablized at 40 DEG C, 150 parts of formaldehyde are added, controller for water boiler temperature rises, and rises it automatically
Temperature；
(3) when its temperature rises to 60 DEG C, 50 parts of bio-extracts and 60 parts of water are added, and continue to heat up；
(4) control reaction rises to 90 DEG C in 50min, and starts to keep the temperature at this temperature, and detects and glue for 4 glasss of painting at 40 DEG C
Degree；
(5) when its viscosity is in 15.5s or so, starting cooling discharge, reaction was completed, detects it when being finally cooled to 40 DEG C
Viscosity is 17.3s.
The preparation of 1 phenolic resin adhesive of comparative example
(1) first 50 parts of phenol and 15 parts of catalyst are added in reaction kettle, starting stirring is uniformly mixed bottom reactant,
Then reaction system is warming up to 50 DEG C, keeps the temperature 30min at this temperature；
(2) using pump is added dropwise with rate of addition appropriate by 14 parts of instillation reaction kettles of first part's formaldehyde, reaction system exists
30min is kept the temperature at a temperature of this, and temperature of reaction system is to slowly warm up to 80 DEG C in 40min later；
(3) using pump is added dropwise with rate of addition appropriate by 50 parts of instillation reaction kettles of second part formaldehyde, reaction system exists
50min is kept the temperature at a temperature of this；
(4) 90min is kept the temperature at 80 DEG C；
(5) using pump is added dropwise with rate of addition appropriate by 10 parts of instillation reaction kettles of Part III formaldehyde, reaction system exists
30min is kept the temperature at a temperature of this；
(6) temperature of reaction system is reduced to 40 DEG C, it is 17.5s that its viscosity is detected when being finally cooled to 40 DEG C.
By phenolic resin adhesive made from modified phenolic resin adhesive made from above-described embodiment 1-3 and comparative example,
It is tested for the property respectively, test result is as follows shown in table 1:
Table 1
| Embodiment | 40 DEG C of paintings, 4 glasss of viscosity s |
| Embodiment 1 | 17 |
| Embodiment 2 | 17.5 |
| Embodiment 3 | 17.3 |
| Comparative example 1 | 17.5 |
From result, embodiment is not much different with comparative example viscosity.But the method for the present invention starts to react in low temperature, easily
Control；System heating is provided by raw material exothermic heat of reaction, can be heated up without heating and be saved the energy；The phenol produced using the present invention
The small bond paper dipping that is more applicable for of urea formaldehyde adhesive molecular weight uses；The present invention is modified using bio-extract, can
To reduce environmental pollution, help is provided to environmental protection.
Specific embodiments of the present invention are described in detail above, but it is merely an example, the present invention is simultaneously unlimited
It is formed on particular embodiments described above.To those skilled in the art, any couple of present invention carries out equivalent modifications and
Substitution is also all among scope of the invention.Therefore, without departing from the spirit and scope of the invention made by equal transformation and
Modification, all should be contained within the scope of the invention.
Claims (8)
1. a kind of preparation method of the modified phenolic resin adhesive suitable for bond paper, which is characterized in that by phenol, catalyst
It is added in reaction kettle, within limits by temperature control, whole formaldehyde, which are added, makes it automatically continuously heat up, and in certain temperature
Degree is lower to be added bio-extract, a period of time is finally reacted at 80~100 DEG C, 4 glasss of viscosity of painting to reaction system are at 40 DEG C
Under when reaching 14~17s, just reaction was completed to get.
2. the preparation method of the modified phenolic resin adhesive according to claim 1 suitable for bond paper, feature exist
According to parts by weight, each raw material dosage is as follows:
3. the preparation method of the modified phenolic resin adhesive according to claim 1 or 2 suitable for bond paper, feature
It is, the temperature when formaldehyde is added in reaction system is 30~50 DEG C.
4. the preparation method of the modified phenolic resin adhesive according to claim 1 or 2 suitable for bond paper, feature
It is, the temperature when bio-extract is added in reaction system is 50~80 DEG C.
5. the preparation method of the modified phenolic resin adhesive according to claim 1 or 2 suitable for bond paper, feature
It is, the temperature at the end of reaction system is reacted is 80~100 DEG C.
6. the preparation method of the modified phenolic resin adhesive according to claim 1 or 2 suitable for bond paper, feature
It is, the catalyst is one or more of barium hydroxide, calcium hydroxide, sodium hydroxide.
7. the preparation method of the modified phenolic resin adhesive according to claim 1 or 2 suitable for bond paper, feature
It is, the bio-extract results from timber, useless selected from paper waste corruption slurry, screenings, bark, medicament waste liquid, grass end, slurrying
One or more of liquid.
8. the preparation method of the modified phenolic resin adhesive according to claim 1 or 2 suitable for bond paper, feature
It is, specifically comprises the following steps:
(1) reaction kettle is first added in phenol, catalyst, stirred；
(2) when temperature is controlled at 30~50 DEG C, formaldehyde is added, starts to control its temperature, makes its automatic heating；
(3) control reaction temperature is warming up to 50~80 DEG C, bio-extract and water is added, and continue to heat up；
(4) control reaction temperature is warming up to 80~100 DEG C, after its temperature is stablized, detects its 4 glasss of viscosity of painting at 40 DEG C；
(5) when viscosity reaches 14~17s, start to cool down, reaction was completed, and detects viscosity when it is cooled to 40 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811574948.2A CN109679044A (en) | 2018-12-21 | 2018-12-21 | A kind of preparation method of the modified phenolic resin adhesive suitable for bond paper |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811574948.2A CN109679044A (en) | 2018-12-21 | 2018-12-21 | A kind of preparation method of the modified phenolic resin adhesive suitable for bond paper |
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| CN109679044A true CN109679044A (en) | 2019-04-26 |
Family
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109456497A (en) * | 2018-10-15 | 2019-03-12 | 昆明荣尊华品木业有限公司 | Resin quick curing method for bond paper dipping |
| CN111944464A (en) * | 2020-07-02 | 2020-11-17 | 上海昶法新材料有限公司 | Modified phenolic resin adhesive and preparation method and application thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109456497A (en) * | 2018-10-15 | 2019-03-12 | 昆明荣尊华品木业有限公司 | Resin quick curing method for bond paper dipping |
| CN109456497B (en) * | 2018-10-15 | 2022-05-17 | 昆明荣尊华品木业有限公司 | Resin rapid curing method for impregnating adhesive film paper |
| CN111944464A (en) * | 2020-07-02 | 2020-11-17 | 上海昶法新材料有限公司 | Modified phenolic resin adhesive and preparation method and application thereof |
| EP3988628A4 (en) * | 2020-07-02 | 2022-09-28 | Shanghai Changfa New Materials Co., Ltd. | Modified phenolic resin adhesive, preparation method therefor and application thereof |
| CN111944464B (en) * | 2020-07-02 | 2023-01-24 | 上海昶法新材料有限公司 | Modified phenolic resin adhesive and preparation method and application thereof |
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