CN108795352A - A kind of preparation method of 0 grade of waterproof floor glue of new E - Google Patents

A kind of preparation method of 0 grade of waterproof floor glue of new E Download PDF

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Publication number
CN108795352A
CN108795352A CN201810789007.4A CN201810789007A CN108795352A CN 108795352 A CN108795352 A CN 108795352A CN 201810789007 A CN201810789007 A CN 201810789007A CN 108795352 A CN108795352 A CN 108795352A
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CN
China
Prior art keywords
urea
reaction kettle
melamine
added
grade
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Pending
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CN201810789007.4A
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Chinese (zh)
Inventor
彭宗军
姜涛
姚加发
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Dalian Kang Neng Coating Co Ltd
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Dalian Kang Neng Coating Co Ltd
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Priority to CN201810789007.4A priority Critical patent/CN108795352A/en
Publication of CN108795352A publication Critical patent/CN108795352A/en
Pending legal-status Critical Current

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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
    • C09J161/00Adhesives based on condensation polymers of aldehydes or ketones; Adhesives based on derivatives of such polymers
    • C09J161/20Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen
    • C09J161/30Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with heterocyclic and acyclic or carbocyclic compounds
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G12/00Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen
    • C08G12/02Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes
    • C08G12/26Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with heterocyclic compounds
    • C08G12/34Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with heterocyclic compounds and acyclic or carbocyclic compounds
    • C08G12/36Ureas; Thioureas
    • C08G12/38Ureas; Thioureas and melamines

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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)
  • Phenolic Resins Or Amino Resins (AREA)

Abstract

The present invention discloses a kind of preparation method of 0 grade of waterproof floor glue of new E, it is characterised in that:The method carries out successively according to the following steps:It is first 2.4-2.5 according to molar ratio by formaldehyde, urea, melamine:1:The ratio of 0.8-0.15, is added in reaction kettle, and synthetic catalyst is added into reaction kettle, and the synthetic catalyst is the 1-1.5% of urea gross mass, and synthetic catalyst by sodium hydroxide and PVA according to mass ratio 1:1 ratio mixes, and the mixture pH value in reaction kettle is adjusted to 7.5-8,30min is kept the temperature after allowing reaction kettle to be warming up to 90-93 DEG C.This is a kind of of low cost, and easy to operate, available stability is good, environmental protection, the method for the E0 grade waterproof floor glue of low price.

Description

A kind of preparation method of 0 grade of waterproof floor glue of new E
Technical field
The present invention relates to a kind of chemical field, especially a kind of preparation method of 0 grade of waterproof floor glue of new E.
Background technology
In the production of China's glued board and solid wooden floor board, adhesive be mainly phenolic resin, Lauxite, isocyanates and Three component solid, powdery glue, wherein three component solid, powdery glue and isocyanates cost are higher, overall cost is in 8000-12000 Yuan/ton, and burst size of methanal is higher.Phenolic resin has excellent handing-over intensity and water resistance, but cured glue layer is at purple Red has base material certain pollution, limits its use scope, overall cost is at 4000-5000 yuan/ton.Though Lauxite So of low cost, for overall cost at 2000-3000 yuan/ton, curing rate is fast, but water resistance is poor, and glue-line is easy to aging, so only The problems such as glued board bonding that can be used for low side uses, and there are serious formaldehyde pollutions.
Used so how to produce and can be used for high-end floor, and cost is relatively low, water resistance and glue-joint strength compared with Height, and there is the adhesive of good environmental-protecting performance to become project.
Invention content
The present invention is to propose that one kind is of low cost to solve the above-mentioned deficiency present in the prior art, easy to operate, can It is good to obtain stability, environmental protection, the method for the E0 grade waterproof floor glue of low price.
Technical solution of the invention is:A kind of preparation method of 0 grade of waterproof floor glue of new E, it is characterised in that:Institute The method stated carries out successively according to the following steps:
A, first by formaldehyde, urea, melamine according to molar ratio be 2.4-2.5:1:The ratio of 0.8-0.15 is added to reaction In kettle, and synthetic catalyst is added into reaction kettle, the synthetic catalyst is the 1-1.5% of urea gross mass, and synthesis is urged Agent is by sodium hydroxide and PVA according to mass ratio 1:1 ratio mixes, by the mixture pH value in reaction kettle adjust to 7.5-8
B, 30min is kept the temperature after allowing reaction kettle to be warming up to 90-93 DEG C,
C, the mixture pH value in reaction kettle is adjusted to 6.5, and urea and melamine is added again into reaction kettle, and urine is added The molar ratio of element and formaldehyde in reaction kettle after melamine, urea, melamine is 1.85-1.95:1:0.1-0.15, allows reaction Temperature in the kettle is maintained at 90-92 DEG C, polycondensation to viscosity terminal,
D, the mixture pH value in reaction kettle is adjusted to 7.5-8.0, and urea and melamine is added for the third time into reaction kettle, Be added after urea and melamine formaldehyde in reaction kettle, urea, melamine molar ratio be 1.45-1.55:1:0.2-0.3,
E, it allows reactor temperature to be maintained at 85 DEG C or more, and keeps the temperature 30min, be then cooled to 45 DEG C, adjust in reaction kettle and mix Object pH value is closed to 7.5-8.0, obtains E0 grades of waterproof floor glue.
In a steps, formaldehyde, urea, melamine molar ratio be 2.44:1:0.11.
In the step c, the molar ratio that urea and formaldehyde in reaction kettle after melamine, urea, melamine is added is 1.91:1:0.13。
In the Step d, the molar ratio that urea and formaldehyde in reaction kettle after melamine, urea, melamine is added is 1.49:1:0.25。
In a steps, synthetic catalyst is the 1.2% of urea gross mass.
The present invention compared with the existing technology, has the following advantages that:
The preparation method of this kind of waterproof floor glue, introduces melamine in technical process, although increasing to a certain extent Original cost, but overall cost is still under three component solid, powdery glue and isocyanates, face suitable with phenolic resin cost Color is creamy white, pollution-free to base material.And in glue-joint strength and water resistance, melamine copolymeric condensation is introduced, is formed three-dimensional Reticular structure encloses hydrophilic radical, while reducing degradation and the hydrolysis rate of resin, improves water resistance and is glued strong Degree.Also increase its stability simultaneously, extends shelf life.In terms of environmental protection, introduce melamine reduces formaldehyde and urea first Molar ratio, while melamine can be reacted with formaldehyde copolymer, generated melamine methylol, contained to drop low-free formaldehyde Amount.In summary, it may be said that the waterproof floor glue that this method prepares has a variety of advantages, particularly suitable in ability It is promoted and applied in domain, market prospects are very wide.
Specific implementation mode
The specific implementation mode of the present invention is described below.A kind of preparation method of 0 grade of waterproof floor glue of new E, according to Following steps carry out successively:
It is first 2.4-2.5 according to molar ratio by formaldehyde, urea, melamine:1:The ratio of 0.8-0.15, is added to reaction kettle In, aforementioned proportion is preferably 2.44:1:0.11;And synthetic catalyst is added into reaction kettle, the synthetic catalyst is urine The 1-1.5% of plain gross mass, preferably 1.2%;And synthetic catalyst by sodium hydroxide and PVA according to mass ratio 1:1 ratio is mixed It closes, the mixture pH value in reaction kettle is adjusted to 7.5-8,
Then, 30min is kept the temperature after allowing reaction kettle to be warming up to 90-93 DEG C,
Next, the mixture pH value in adjustment reaction kettle and urea and melamine is added into reaction kettle again to 6.5, Be added after urea and melamine formaldehyde in reaction kettle, urea, melamine molar ratio be 1.85-1.95:1:0.1-0.15, Aforementioned proportion is preferably 1.91:1:0.13, allow reactor temperature to be maintained at 90-92 DEG C, polycondensation to viscosity terminal,
Then the mixture pH value in reaction kettle is adjusted to 7.5-8.0, and urea and melamine is added for the third time into reaction kettle Amine, be added after urea and melamine formaldehyde in reaction kettle, urea, melamine molar ratio be 1.45-1.55:1:0.2- 0.3, aforementioned proportion is preferably 1.49:1:0.25;
Finally, it allows reactor temperature to be maintained at 85 DEG C or more, and keeps the temperature 30min, be then cooled to 45 DEG C, adjust in reaction kettle Mixture pH value obtains E0 grades of waterproof floor glue to 7.5-8.0.
Using the E0 grade waterproof floor glue prepared by this method, compareed with traditional floor glue performance:
One, physical index
Viscosity is measured using applying -4 glasss 25 degree.
Solid content is measured using drying box method.
Storage time is calculated according to viscosity and bonding force variation
Performance table
Two, overall cost compares
Cost and comparison
Comparative illustration, it is minimum in the E0 grade waterproof floor glue costs used suitable for floor, and environmental protection grade highest, while it is right Base material is pollution-free.
Three, water boiling resistance Experimental comparison
Model acquires:
Three layers of composite floor board of solid wood.
By every square meter 360g or so glue-spread brushing.
E0 grades of waterproof floor glue are using cold pressing 30min, and hot pressing 105 degree of 7min are quiet to put 3 hours.
Use 80 degree of its water boiling resistance times of measurement of thermostat water bath.
Water boiling resistance is tested
Experiment shows that E0 grades of waterproof floor glue since NPVA and melamine are introduced, have excellent water resistance, with phenolic aldehyde tree Lipid phase is worked as, and boiling is more than 3 hours not have any cracking phenomena in 80 degree of water.
Four, environmental protection grade
Burst size of methanal:40L condensed steam waters
Experiment shows that E0 grades of its process modification of waterproof floor glue are introduced with melamine, so that burst size of methanal is preferably minimized, reaches The world requires most stringent of Japan F4 stars to require.

Claims (5)

1. a kind of preparation method of 0 grade of waterproof floor glue of new E, it is characterised in that:The method is according to the following steps successively It carries out:
A, first by formaldehyde, urea, melamine according to molar ratio be 2.4-2.5:1:The ratio of 0.8-0.15 is added to reaction In kettle, and synthetic catalyst is added into reaction kettle, the synthetic catalyst is the 1-1.5% of urea gross mass, and synthesis is urged Agent is by sodium hydroxide and PVA according to mass ratio 1:1 ratio mixes, by the mixture pH value in reaction kettle adjust to 7.5-8
B, 30min is kept the temperature after allowing reaction kettle to be warming up to 90-93 DEG C,
C, the mixture pH value in reaction kettle is adjusted to 6.5, and urea and melamine is added again into reaction kettle, and urine is added The molar ratio of element and formaldehyde in reaction kettle after melamine, urea, melamine is 1.85-1.95:1:0.1-0.15, allows reaction Temperature in the kettle is maintained at 90-92 DEG C, polycondensation to viscosity terminal,
D, the mixture pH value in reaction kettle is adjusted to 7.5-8.0, and urea and melamine is added for the third time into reaction kettle, Be added after urea and melamine formaldehyde in reaction kettle, urea, melamine molar ratio be 1.45-1.55:1:0.2-0.3,
E, it allows reactor temperature to be maintained at 85 DEG C or more, and keeps the temperature 30min, be then cooled to 45 DEG C, adjust in reaction kettle and mix Object pH value is closed to 7.5-8.0, obtains E0 grades of waterproof floor glue.
2. the preparation method of 0 grade of waterproof floor glue of new E according to claim 1, it is characterised in that:In a steps, Formaldehyde, urea, melamine molar ratio be 2.44:1:0.11.
3. the preparation method of 0 grade of waterproof floor glue of new E according to claim 1, it is characterised in that:In the step c, Be added after urea and melamine formaldehyde in reaction kettle, urea, melamine molar ratio be 1.91:1:0.13.
4. the preparation method of 0 grade of waterproof floor glue of new E according to claim 1, it is characterised in that:In the Step d, Be added after urea and melamine formaldehyde in reaction kettle, urea, melamine molar ratio be 1.49:1:0.25.
5. the preparation method of 0 grade of waterproof floor glue of new E according to claim 1, it is characterised in that:In a steps, Synthetic catalyst is the 1.2% of urea gross mass.
CN201810789007.4A 2018-07-18 2018-07-18 A kind of preparation method of 0 grade of waterproof floor glue of new E Pending CN108795352A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2023094603A1 (en) 2021-11-25 2023-06-01 Foresa Technologies, S.L.U. Method for the production of melamine-urea-formaldehyde resins, the resins obtained therewith, and applications of said resins

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2002097434A (en) * 2000-09-21 2002-04-02 Sumitomo Bakelite Co Ltd Adhesive for producing odorless wooden board
CN101244571A (en) * 2008-03-21 2008-08-20 中国林业科学研究院林产化学工业研究所 Method for manufacturing E0 level wood veneer
CN102775571A (en) * 2012-07-23 2012-11-14 中国林业科学研究院林产化学工业研究所 Method for preparing melamine-urea-formaldehyde resin adhesives for outdoor plywood low in formaldehyde release

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2002097434A (en) * 2000-09-21 2002-04-02 Sumitomo Bakelite Co Ltd Adhesive for producing odorless wooden board
CN101244571A (en) * 2008-03-21 2008-08-20 中国林业科学研究院林产化学工业研究所 Method for manufacturing E0 level wood veneer
CN102775571A (en) * 2012-07-23 2012-11-14 中国林业科学研究院林产化学工业研究所 Method for preparing melamine-urea-formaldehyde resin adhesives for outdoor plywood low in formaldehyde release

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
王巍: "E0级胶合板用脲醛树脂胶黏剂的研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2023094603A1 (en) 2021-11-25 2023-06-01 Foresa Technologies, S.L.U. Method for the production of melamine-urea-formaldehyde resins, the resins obtained therewith, and applications of said resins

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Application publication date: 20181113