CN101481445B - Melamine-formaldehyde impregnating resin and preparing method thereof - Google Patents
Melamine-formaldehyde impregnating resin and preparing method thereof Download PDFInfo
- Publication number
- CN101481445B CN101481445B CN2009100255014A CN200910025501A CN101481445B CN 101481445 B CN101481445 B CN 101481445B CN 2009100255014 A CN2009100255014 A CN 2009100255014A CN 200910025501 A CN200910025501 A CN 200910025501A CN 101481445 B CN101481445 B CN 101481445B
- Authority
- CN
- China
- Prior art keywords
- formaldehyde
- correcting agent
- properties
- temperature
- value
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Abstract
The invention discloses a melamine-formaldehyde dipping resin which consists of 34-45 percent of formaldehyde, 30-40 percent of melamine, 1-4 percent of diethylene glycol, 12-28 percent of purified water, 1-4 percent of modifying agent and sodium hydroxide according to weight percentage; the invention further discloses a preparation method of the melamine-formaldehyde dipping resin. Caprolactam is omitted in the raw material formulation; by changing the formulation of raw material composition, each performance index of the polymer resin, which is finally generated, meets each index requirement of the dipping resin; when the dipping resin is used for manufacturing laminated flooring, the detected performance indexes of the flooring also meet the quality index requirements. As the caprolactam is omitted in the raw material formulation, production cost is greatly saved and process steps are simplified.
Description
Technical field
The present invention relates to a kind of resin and manufacture method thereof, particularly a kind of melamine formaldehyde resin also relates to the manufacture method of this resin, and this resin can be used to flood abrasion-proof paper, decorative paper and the balance paper of laminate flooring simultaneously.
Background technology
Laminated flooring adds general abrasion-proof paper, decorative paper and the balance paper that adopts melamine formaldehyde resin dipping laminate flooring in man-hour, then these three impregnated papers is overlayed on base material with low pressure short period press, thereby forms the dipping laminate flooring.The carbamide solvent impregnated resin be by trimeric cyanamide and formaldehyde under alkaline condition, addition reaction taking place generates melamine methylol, and then forms resin.But the resin fragility of condition formation is bigger like this, need just can be used for the production of laminated wood floor impregnated paper under the condition of High Temperature High Pressure.Some modified cyanurotriamide-formaldehyde resins have appearred at present, to adapt to enterprise uses low pressure short period press when producing laminated wood floor actual needs.Many when actual production carbamide solvent impregnated resin is raw material with formaldehyde, trimeric cyanamide, pure water, hexanolactam, Diethylene Glycol, properties-correcting agent and sodium hydroxide, and manufacturing process is that other raw materials such as formaldehyde and trimeric cyanamide aggregate into resin under the condition that Diethylene Glycol and pure water are arranged in weak alkaline medium.Because hexanolactam costs an arm and a leg, and makes that the production cost of carbamide solvent impregnated resin is also very high.
Summary of the invention
The object of the present invention is to provide a kind of carbamide solvent impregnated resin and manufacturing process thereof, this technological operation is simple, production efficiency is high, and the solvent impregnated resin that produces through this technology has advantages such as cost is low, suitability wide, excellent property.
The present invention is achieved by the following technical programs.
A kind of carbamide solvent impregnated resin, form by formaldehyde, trimeric cyanamide, Diethylene Glycol, pure water, properties-correcting agent and sodium hydroxide, their weight percent consists of: the formaldehyde of 35-45%, the trimeric cyanamide of 30-40%, the Diethylene Glycol of 1-4%, the pure water of 12-28%, the properties-correcting agent of 1-4%, surplus is a sodium hydroxide.
The manufacturing process of above-mentioned a kind of carbamide solvent impregnated resin, it comprises the steps:
A, cleaning reaction still are closed bottom valve;
B, in reactor, add the pure water that weight percent is 12-28%, the formaldehyde of 35-45%, the Diethylene Glycol of 1-4% and the properties-correcting agent of 1-4% successively, and stir and add proper amount of sodium hydroxide solution and regulate pH value to 8.5～9.5;
C, adding weight percent are the trimeric cyanamide of 30-40% and stirred 10 minutes;
D, intensification rose to 85～95 ℃ with temperature in 30～40 minutes;
E, the hierarchy of control are that 85～95 ℃, pH value are to react 30min, the water-soluble multiple of the detection reaction of taking a sample then liquid under 8.5～9.5 the state in temperature;
F, when water-soluble multiple reach 1: 1.5～2.5 the time, cooling rapidly;
G, when temperature is reduced to below 30 ℃, regulating pH value is 8.5～9.6, then sampling, discharging.
The trade name of employed properties-correcting agent is cyanurotriamide modified dose of MF-1 in the raw material of the present invention, and its main component is dibasic alcohol (1, the 4-butyleneglycol), polyol ethers, polyvalent alcohol (sorbyl alcohol) and para toluene sulfonamide.This properties-correcting agent can make resin flowability, toughness, the glossiness of glued membrane, the compactness of glued membrane and the stability in storage of resin etc. under low pressure all improve.
Contain this composition of hexanolactam in the raw material of prior art production carbamide solvent impregnated resin, using the effect of hexanolactam is in order to improve the toughness of polymer resin, there is not hexanolactam in the raw materials for production of carbamide solvent impregnated resin of the present invention, the present invention makes every performance index of the final polymer resin that generates all reach every index request of solvent impregnated resin by changing the proportioning of various feed composition.Owing to saved this composition of hexanolactam in the composition of raw materials,, also simplified processing step simultaneously so saved production cost greatly.And carbamide solvent impregnated resin of the present invention can be used to flood abrasion-proof paper, decorative paper and the balance paper of laminate flooring simultaneously, do not need to produce the resin of other kinds again, thereby saved resource and energy consumption, improved production efficiency, reduced cost.
Embodiment
Raw material:
Formaldehyde: purity 37.2%, liquid; Trimeric cyanamide: purity 99.8%, white crystal; Diethylene Glycol: purity 99%, liquid; Sodium hydroxide: purity 30%, liquid.Properties-correcting agent: trade name is cyanurotriamide modified dose of MF-1, and purity 73% is purchased in Chengdu Yong Gang tiger king finishing material company limited, and main component is dibasic alcohol (1, the 4-butyleneglycol), polyol ethers, polyvalent alcohol (sorbyl alcohol) and para toluene sulfonamide.
Embodiment 1
Pure water with 3500kg, the formaldehyde of 7500kg, the Diethylene Glycol of 600kg and the properties-correcting agent of 720kg add in the reactor successively, stir the sodium hydroxide solution that adds 7L and regulate pH value to 9.23, add the trimeric cyanamide of 6800kg then and stirred 10 minutes, in 30 minutes, temperature is risen to 90.1 ℃, the hierarchy of control is 90.1 ℃ in temperature, the pH value is 9.23 the following reaction of state 30min, the water-soluble multiple of the detection reaction of taking a sample then liquid, when reaching 2.5, water-soluble multiple lowers the temperature rapidly, when temperature is reduced to below 30 ℃, regulating the pH value is 8.92, then sampling, discharging.
Every detected result
Index is detected on the floor:
Embodiment 2
With the pure water of 3274kg, the formaldehyde of 6100kg, the Diethylene Glycol of 400kg and the properties-correcting agent of 600kg add in the reactor successively, stir the sodium hydroxide solution that adds 8L and regulate pH value to 9.5, add the trimeric cyanamide of 5426kg then and stirred 10 minutes, in 40 minutes, temperature is risen to 85 ℃, the hierarchy of control is that 85 ℃, pH value are to react 30min under 9.5 the state in temperature, the water-soluble multiple of the detection reaction of taking a sample then liquid, when reaching 1.7, water-soluble multiple lowers the temperature rapidly, when temperature is reduced to below 30 ℃, regulating the pH value is 9.6, then sampling, discharging.
Every detected result
| Test item | Quality index | Detected result |
| Outward appearance | Colourless transparent liquid | Colourless transparent liquid |
| The pH value | 8.5-9.6 | 9.5 |
| Viscosity (s/20 ℃) is coated with the 4# cup | 15-25 | 17 |
| Solid content (wt%) | 45-60 | 53.9 |
| Water-soluble multiple (25 ℃) | 1.5-2.5 | 1.6 |
| Free formaldehyde (wt%) | ≤0.3 | 0.2 |
Index is detected on the floor:
Embodiment 3
Pure water with 1990kg, the formaldehyde of 7290kg, the Diethylene Glycol of 324kg and the properties-correcting agent of 162kg add in the reactor successively, stir the sodium hydroxide solution that adds 7L and regulate pH value to 9.26, add the trimeric cyanamide of 6434kg then and stirred 10 minutes, in 30 minutes, temperature is risen to 90.1 ℃, the hierarchy of control is 90.1 ℃ in temperature, the pH value is 9.26 the following reaction of state 30min, the water-soluble multiple of the detection reaction of taking a sample then liquid, when reaching 2.5, water-soluble multiple lowers the temperature rapidly, when temperature is reduced to below 30 ℃, regulating the pH value is 8.97, then sampling, discharging.
Every detected result
| Test item | Quality index | Detected result |
| Outward appearance | Colourless transparent liquid | Colourless transparent liquid |
| The pH value | 8.5-9.6 | 9.0 |
| Viscosity (s/20 ℃) is coated with the 4# cup | 15-25 | 18 |
| Solid content (wt%) | 45-60 | 59 |
| Water-soluble multiple (25 ℃) | 1.5-2.5 | 1.9 |
| Free formaldehyde (wt%) | ≤0.3 | 0.3 |
Index is detected on the floor:
Embodiment 4
Pure water with 2785kg, the formaldehyde of 6966kg, the Diethylene Glycol of 162kg and the properties-correcting agent of 162kg add in the reactor successively, stir the sodium hydroxide solution that adds 7L and regulate pH value to 9.25, add the trimeric cyanamide of 6125kg then and stirred 10 minutes, in 30 minutes, temperature is risen to 90.2 ℃, the hierarchy of control is 90.2 ℃ in temperature, the pH value is 9.25 the following reaction of state 30min, the water-soluble multiple of the detection reaction of taking a sample then liquid, when reaching 1.5, water-soluble multiple lowers the temperature rapidly, when temperature is reduced to below 30 ℃, regulating the pH value is 8.95, then sampling, discharging.
Every detected result
| Test item | Quality index | Detected result |
| Outward appearance | Colourless transparent liquid | Colourless transparent liquid |
| The pH value | 8.5-9.6 | 9.0 |
| Viscosity (s/20 ℃) is coated with the 4# cup | 15-25 | 17 |
| Solid content (wt%) | 45-60 | 55.4 |
| Water-soluble multiple (25 ℃) | 1.5-2.5 | 1.5 |
| Free formaldehyde (wt%) | ≤0.3 | 0.3 |
Index is detected on the floor:
Embodiment 5
With the pure water of 4450kg, the formaldehyde of 5775kg, the Diethylene Glycol of 510kg and the properties-correcting agent of 510kg add in the reactor successively, stir the sodium hydroxide solution that adds 7L and regulate pH value to 8.5, add the trimeric cyanamide of 5250kg then and stirred 10 minutes, in 30 minutes, temperature is risen to 95 ℃, the hierarchy of control is that 95 ℃, pH value are to react 30min under 8.5 the state in temperature, the water-soluble multiple of the detection reaction of taking a sample then liquid, when reaching 2.5, water-soluble multiple lowers the temperature rapidly, when temperature is reduced to below 30 ℃, regulating the pH value is 8.5, then sampling, discharging.
Every detected result
| Test item | Quality index | Detected result |
| Outward appearance | Colourless transparent liquid | Colourless transparent liquid |
| The pH value | 8.5-9.6 | 8.5 |
| Viscosity (s/20 ℃) is coated with the 4# cup | 15-25 | 16 |
| Solid content (wt%) | 45-60 | 50.1 |
| Water-soluble multiple (25 ℃) | 1.5-2.5 | 2.1 |
| Free formaldehyde (wt%) | ≤0.3 | 0.2 |
Index is detected on the floor:
Can find out by the foregoing description, do not use this composition of hexanolactam in the raw material of the present invention, but every performance index of the carbamide solvent impregnated resin of finally making such as outward appearance, viscosity, solid content etc. have all reached the quality index requirement of solvent impregnated resin in the actual production, when simultaneously solvent impregnated resin of the present invention being used to produce laminated flooring, every performance of laminated flooring has also all reached the quality index requirement.
Here description of the invention and application is illustrative, is not to want that therefore, the present invention is not subjected to the restriction of present embodiment with scope restriction of the present invention in the above-described embodiments, and the technical scheme that any employing equivalence replacement obtains is all in the scope of protection of the invention.
Claims (2)
1. carbamide solvent impregnated resin, it is characterized in that, prepare by formaldehyde, trimeric cyanamide, Diethylene Glycol, pure water, properties-correcting agent and sodium hydroxide, their weight percent consists of: the formaldehyde of 35-45%, the trimeric cyanamide of 30-40%, the Diethylene Glycol of 1-4%, the pure water of 12-28%, the properties-correcting agent of 1-4%, surplus is a sodium hydroxide, the trade name of described properties-correcting agent is cyanurotriamide modified dose of MF-1, and its main component is a dibasic alcohol 1,4-butyleneglycol, polyol ethers, polyvalent alcohol sorbyl alcohol and para toluene sulfonamide.
2. the manufacture method of a kind of carbamide solvent impregnated resin as claimed in claim 1 is characterized in that, comprises the steps:
A, cleaning reaction still are closed bottom valve;
B, in reactor, add the pure water that weight percent is 12-28%, the formaldehyde of 35-45%, the Diethylene Glycol of 1-4% and the properties-correcting agent of 1-4% successively, and stir adding proper amount of sodium hydroxide solution and regulate pH value to 8.5～9.5, the trade name of described properties-correcting agent is cyanurotriamide modified dose of MF-1, its main component is a dibasic alcohol 1,4-butyleneglycol, polyol ethers, polyvalent alcohol sorbyl alcohol and para toluene sulfonamide;
C, adding weight percent are the trimeric cyanamide of 30-40% and stirred 10 minutes;
D, in 30～40 minutes, temperature is risen to 85～95 ℃;
E, the hierarchy of control are that 85～95 ℃, pH value are to react 30min, the water-soluble multiple of the detection reaction of taking a sample then liquid under 8.5～9.5 the state in temperature;
F, when water-soluble multiple reach 1: 1.5～2.5 the time, cooling rapidly;
G, when temperature is reduced to below 30 ℃, regulating pH value is 8.5～9.6, takes a sample then, discharging.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009100255014A CN101481445B (en) | 2009-02-06 | 2009-02-06 | Melamine-formaldehyde impregnating resin and preparing method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009100255014A CN101481445B (en) | 2009-02-06 | 2009-02-06 | Melamine-formaldehyde impregnating resin and preparing method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101481445A CN101481445A (en) | 2009-07-15 |
| CN101481445B true CN101481445B (en) | 2011-03-30 |
Family
ID=40878745
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2009100255014A Active CN101481445B (en) | 2009-02-06 | 2009-02-06 | Melamine-formaldehyde impregnating resin and preparing method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101481445B (en) |
Families Citing this family (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101830023A (en) * | 2010-05-14 | 2010-09-15 | 程国凉 | Manufacture process of high-density bamboo chip plates |
| CN102492385A (en) * | 2011-11-28 | 2012-06-13 | 天津市中源装饰材料有限公司 | Melamino-formaldehyde resin adhesive and preparation method |
| CN103172813A (en) * | 2013-03-27 | 2013-06-26 | 湖南福湘木业有限责任公司 | Melamine formaldehyde resin and synthesis technology thereof |
| CN104559873A (en) * | 2013-10-22 | 2015-04-29 | 寿光市东宇鸿翔木业有限公司 | Melamine glue and preparation method thereof |
| CN103980448B (en) * | 2014-05-30 | 2016-01-13 | 崇州合瑞科技有限公司 | A kind of melamine resin modifier |
| CN105367729A (en) * | 2015-11-03 | 2016-03-02 | 湖北鸿连实业有限公司 | Low-cost high-tension modified melamine-formaldehyde resin for equilibrium paper and preparation method thereof |
| CN106243911B (en) * | 2016-07-29 | 2018-09-25 | 神盾防火科技有限公司 | It is used to prepare the preparation and application of the resin combination of fiber fire-proof and thermal-insulation coating |
| CN107177027A (en) * | 2017-06-01 | 2017-09-19 | 东莞市贝辉装饰材料有限公司 | A kind of cyanurotriamide modified resin and its preparation method and application |
| CN107474206A (en) * | 2017-08-10 | 2017-12-15 | 浙江宜佳新材料股份有限公司 | A kind of preparation technology of high-ductility melamine resin |
| CN108687887A (en) * | 2018-04-23 | 2018-10-23 | 太尔化工（南京）有限公司 | A kind of preparation method and application of solid-state bloom melamine-impregnated decorative paper |
| CN109354661A (en) * | 2018-10-15 | 2019-02-19 | 昆明荣尊华品木业有限公司 | A kind of bond paper dip resin modifying agent and preparation method thereof |
| CN109403139A (en) * | 2018-11-08 | 2019-03-01 | 河北盛林装饰纸有限公司 | A kind of production method of impregnating resin and bloom impregnated bond paper |
| CN110499673A (en) * | 2019-08-27 | 2019-11-26 | 江苏美新建材科技有限公司 | A kind of decoration composite faced plywood bent |
| CN110509649A (en) * | 2019-08-29 | 2019-11-29 | 安徽扬子地板股份有限公司 | Floor a kind of high thermal stability SPC and preparation method thereof |
| CN111730697B (en) * | 2020-07-08 | 2022-04-19 | 百草边大生物科技(青岛)有限公司 | Wormwood modified veneer and preparation method thereof |
| CN113389347B (en) * | 2021-07-14 | 2022-12-20 | 德尔未来科技控股集团股份有限公司 | High-simulation digitally-printed decorative paper laminate wood floor and preparation method thereof |
| CN113524936A (en) * | 2021-07-14 | 2021-10-22 | 德尔未来科技控股集团股份有限公司 | Preparation method, product and application of high-simulation digital printing impregnated bond paper |
-
2009
- 2009-02-06 CN CN2009100255014A patent/CN101481445B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN101481445A (en) | 2009-07-15 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101481445B (en) | Melamine-formaldehyde impregnating resin and preparing method thereof | |
| CN102604573A (en) | E0-grade melamine modified urea-formaldehyde resin adhesive, and preparation method and application thereof | |
| CN102604021B (en) | Method for synthesizing urea-formaldehyde resin containing micro free formaldehyde for E0-level artificial boards | |
| CN102977846B (en) | Adhesive for plywood and method for preparing same | |
| CN102134468A (en) | Method for preparing adhesive for grade-E0 medium density fiberboards | |
| CN101817913A (en) | Preparation method of highly methyl etherified amino resin | |
| CN102408855A (en) | Urea formaldehyde resin adhesive for moisture-proof environment-friendly medium density fiberboard and production method as well as composite additives thereof | |
| CN113322024B (en) | Composite water-based crosslinking modifier and preparation method and application thereof | |
| CN103666348A (en) | Highly-dampproof adhesive and preparation method thereof | |
| CN105504193B (en) | Moisture-proof environment-friendlyshoe cyanurotriamide modified urea resin adhesive and preparation method thereof | |
| CN110734735B (en) | High-branched polymer wood adhesive and preparation method and application thereof | |
| CN101786995A (en) | Method for preparing granular hexamethylol melamine | |
| CN102304337A (en) | Novel environmental-friendly modified glue for impregnated paper and preparation method thereof | |
| CN105647449B (en) | A kind of phenol-dialdehyde starch-formaldehyde resin gluing agent and preparation method thereof | |
| CN104910842B (en) | Preparation method of resorcinol modified urea-formaldehyde resin adhesive | |
| CN114134751A (en) | Novel waterproof composite resin for impregnating surface layer of laminate wood floor and preparation method thereof | |
| CN103965425A (en) | Preparation method for water-glass modified amino resin | |
| CN101698786A (en) | Adhesive for orienting shaving board and production method thereof | |
| CN107603541B (en) | A kind of highly filled environmentally friendly condensation copolymerization resin wood adhesive and the preparation method and application thereof | |
| CN107722208A (en) | A kind of environment-friendly type condensation copolymerization resin wood adhesive and preparation method and application | |
| CN103804710A (en) | Preparation method for foam material containing low-hydroxymethyl melamine-formaldehyde resin | |
| CN104559828A (en) | Emulsion paraffin water-proofing agent for particleboard | |
| CN104493948A (en) | Preparation method for shaving board with high moisture content | |
| CN103951806A (en) | Low molecular weight phenolic resin impregnation liquid for manufacturing sticky membrane paper and preparation method of low molecular weight phenolic resin impregnation liquid | |
| CN103788909A (en) | Preparation method of adhesive for E0 environment-friendly shaving board |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |