CN104927012B - Preparation method of water-soluble urea-formaldehyde resin immersion liquid - Google Patents
Preparation method of water-soluble urea-formaldehyde resin immersion liquid Download PDFInfo
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- CN104927012B CN104927012B CN201410549137.2A CN201410549137A CN104927012B CN 104927012 B CN104927012 B CN 104927012B CN 201410549137 A CN201410549137 A CN 201410549137A CN 104927012 B CN104927012 B CN 104927012B
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Abstract
The invention discloses a preparation method of water-soluble urea-formaldehyde resin immersion liquid. The method disclosed by the invention comprises the following steps of: adding 100mol of methanal and 5-30mol of methanol to a reaction kettle, raising temperature to 35-40 DEG C, and adding phosphoric acid, sulphuric acid or acetic acid so as to regulate the pH to 1-3; adding urea for the first time, maintaining the temperature to be 35-40 DEG C, and performing a reaction for 30-50min at the temperature of 35-40 DEG C; adding 5-30mol of melamine, and performing a reaction for 8-20min at the temperature of 35-40 DEG C; adding the urea for the second time, and performing the reaction for 25-40min at the temperature of 35-40 DEG C; adding sodium hydroxide so as to regulate the pH value to 8-10, raising the temperature to 70-85 DEG C, performing the reaction for 40-60min, cooling the reactant, and discharging the cooled reactant. The preparation method disclosed by the invention is simple and practicable, and the production cost is low; the obtained products are good in water solubility, are high in stability and are low in free formaldehyde content.
Description
Technical field
The present invention relates to the preparation method of a kind of Lauxite, particularly to the preparation method of a kind of water-soluble urea-formaldehyde resin impregnation liquid.
Background technology
The advantages such as existing Wooden modifying impregnation liquid, is mostly low-molecular-weight Lauxite or phenolic resin, and Lauxite impregnation liquid has low cost, raw material sources enriches.But it is high to there is also the product burst size of methanal made, not environmentally, preserve short, reusability is poor (can progressively auto polymerization, solidification) thus causes the defects such as production cost is high.Additionally, such Wood modifier needs when using energy consumption and production cost will to be caused high by impregnation processability after timber stoving (water content is less than 20%).
General Lauxite impregnation liquid generally uses alkali-Acid-Base production technology, and the reaction temperature of its acidic phase is generally about 80 DEG C, and pH value is about 6, the condensation reaction between the most multiple methylolurea and carbamide, and production cost is higher.Additionally, the Lauxite impregnation liquid free formaldehyde content being achieved in that is high, water proofing property and stability are the best.
Summary of the invention
It is an object of the invention to provide the preparation method of a kind of water-soluble urea-formaldehyde resin impregnation liquid, simple, production cost is low, products obtained therefrom good water solubility, good stability, and free formaldehyde content is low.
The technical solution adopted for the present invention to solve the technical problems is:
The preparation method of a kind of water-soluble urea-formaldehyde resin impregnation liquid, adds reactor by formaldehyde 100mol and methanol 5-30mol, is warming up to 35-40 DEG C, adding phosphoric acid, sulphuric acid or acetic acid adjusts pH to be 1-3, adds carbamide for the first time, reacts 30-50min at a temperature of being maintained at 35-40 DEG C, add tripolycyanamide 5-30mol, reacting 8-20min at 35-40 DEG C, second time adds carbamide, reacts 25-40min at 35-40 DEG C, hydro-oxidation sodium adjusts pH value 8-10, it is warming up to 70-85 DEG C of reaction 40-60min, cooling, discharging.
As preferably, the amount adding carbamide for the first time is 15-16.7mol.
As preferably, add carbamide for the first time and the total amount adding carbamide for the second time is 90-110mol.
The present invention uses Acid-Base production technology to prepare water-soluble urea-formaldehyde resin impregnation liquid, and use low temperature (35-40 DEG C), highly acid (PH1-3) condition at acidic phase, main purpose is to generate the cyclic compound of part Uron ring (oxa--3,5-phenodiazine cyclohexyl-4-ketone).Cyclic compound good waterproof performance, good stability, and cyclic compound easily infiltrate into wood internal.The purpose adding methanol is to generate part ether-containing key compound, increases bin stability.The purpose adding tripolycyanamide is: make tripolycyanamide and carbamide, formaldehyde condensation copolymerization, improves the resistance to water of resin.
The carbamide of the present invention adds at twice, the most a small amount of addition, and second time is a large amount of to add, such purpose is: is added to part for the first time on a small quantity and forms cyclic compound (Uron ring), cyclic compound good waterproof performance, good stability, and cyclic compound easily infiltrate into wood internal.Second time adds carbamide and generates chain compound, and such production cost is low, and the time is short.Carbamide can not add for the first time in a large number, it is impossible to produces cyclic compound in a large number, and carbamide adds membership for the first time in a large number and causes energy consumption high, and the time is long, and production cost is high.
The invention has the beneficial effects as follows:
1, simple, production cost is low, is suitable for industrialized production.
2, Acid-Base production technology is used to prepare water-soluble urea-formaldehyde resin impregnation liquid, and use low temperature (35-40 DEG C), highly acid (PH1-3) condition at acidic phase, main purpose is to generate the cyclic compound of part Uron ring (oxa--3,5-phenodiazine cyclohexyl-4-ketone).Cyclic compound good waterproof performance, good stability, and cyclic compound easily infiltrate into wood internal.
3, the carbamide of the present invention adds at twice, the most a small amount of addition, and second time is a large amount of to add, and can partly form cyclic compound (Uron ring), and the time is short, low cost.
Detailed description of the invention
Below by specific embodiment, technical scheme is described in further detail.
In the present invention, if not refering in particular to, the raw material used and equipment etc. are all commercially available or commonly used in the art.Method in following embodiment, if no special instructions, is the conventional method of this area.
Embodiment 1:
The preparation method of a kind of water-soluble urea-formaldehyde resin impregnation liquid, adds reactor by formaldehyde 100mol and methanol 5mol, is warming up to 35 DEG C, adding acetic acid adjusts pH to be 3, adds carbamide 15mol for the first time, reacts 50min at a temperature of being maintained at 35 DEG C, add tripolycyanamide 5mol, reacting 20min at 35 DEG C, second time adds carbamide 75mol, reacts 40min at 35 DEG C, hydro-oxidation sodium adjusts pH value 10, it is warming up to 70 DEG C of reaction 60min, cooling, discharging.
Embodiment 2:
The preparation method of a kind of water-soluble urea-formaldehyde resin impregnation liquid, adds reactor by formaldehyde 100mol and methanol 30mol, is warming up to 40 DEG C, adding phosphoric acid adjusts pH to be 1, adds carbamide 16.7mol for the first time, reacts 30min at a temperature of being maintained at 40 DEG C, add tripolycyanamide 30mol, reacting 8min at 40 DEG C, second time adds carbamide 93.3mol, reacts 25min at 40 DEG C, hydro-oxidation sodium adjusts pH value 8, it is warming up to 85 DEG C of reaction 40min, cooling, discharging.
Embodiment 3:
The preparation method of a kind of water-soluble urea-formaldehyde resin impregnation liquid, adds reactor by formaldehyde 100mol and methanol 15mol, is warming up to 40 DEG C, adding sulphuric acid adjusts pH to be 2, adds carbamide 16mol for the first time, reacts 40min at a temperature of being maintained at 40 DEG C, add tripolycyanamide 15mol, reacting 10min at 40 DEG C, second time adds carbamide 84mol, reacts 30min at 40 DEG C, hydro-oxidation sodium adjusts pH value 9, it is warming up to 75 DEG C of reaction 50min, cooling, discharging.
Gained water-soluble urea-formaldehyde resin impregnation liquid of the present invention, its solid content is at 50-60%.Reaching storage period more than 6 months, without precipitation after preserving 6 months, do not whiten, water dilution reaches more than 2 times.
Use gained water-soluble urea-formaldehyde resin impregnation liquid impregnated plate of the present invention to prepare plywood and carry out performance test:
Detecting free formaldehyde content according to European standard EN 120:1992 perforation method, free formaldehyde reaches E0 level.
Room temperature cold water soak 24h, turnover rate≤5%；70 DEG C of hot-water soak 24h, turnover rate≤10%, leach resistance is good.Turnover rate is calculated as: plywood is dried the weight of the moisture content gained to immersion divided by the weight of plywood before soaking after soaking.
Embodiment described above is the one preferably scheme of the present invention, and the present invention not makees any pro forma restriction, also has other variant and remodeling on the premise of without departing from the technical scheme described in claim.
Claims (1)
1. the preparation method of a water-soluble urea-formaldehyde resin impregnation liquid, it is characterized in that: formaldehyde 100mol and methanol 5-30mol is added reactor, it is warming up to 35-40 DEG C, adding phosphoric acid, sulphuric acid or acetic acid adjusts pH to be 1-3, add carbamide for the first time, 30-50min is reacted at a temperature of being maintained at 35-40 DEG C, add tripolycyanamide 5-30mol, reacting 8-20min at 35-40 DEG C, second time adds carbamide, reacts 25-40min at 35-40 DEG C, hydro-oxidation sodium adjusts pH value 8-10, it is warming up to 70-85 DEG C of reaction 40-60min, cooling, discharging；The amount adding carbamide for the first time is 15-16.7mol, and the total amount that addition carbamide and second time add carbamide for the first time is 90-110mol.
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| CN201410549137.2A CN104927012B (en) | 2014-10-16 | 2014-10-16 | Preparation method of water-soluble urea-formaldehyde resin immersion liquid |
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| CN201410549137.2A CN104927012B (en) | 2014-10-16 | 2014-10-16 | Preparation method of water-soluble urea-formaldehyde resin immersion liquid |
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| CN104927012A CN104927012A (en) | 2015-09-23 |
| CN104927012B true CN104927012B (en) | 2017-01-11 |
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| CN106279595A (en) * | 2016-08-01 | 2017-01-04 | 浙江新华新材料科技有限责任公司 | Preparation of urea-formaldehyde resin and Lauxite preparation reactor |
| CN106696018B (en) * | 2016-12-12 | 2018-06-22 | 南京林业大学 | Cottonwood plank stuff impregnates method of modifying |
Citations (6)
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| CN1583815A (en) * | 2004-06-11 | 2005-02-23 | 中国化工建设总公司常州涂料化工研究院 | Preparing method for water soluble urea resin |
| WO2006121352A1 (en) * | 2005-05-11 | 2006-11-16 | Fibre 7 Limited | Wood hardening procedures |
| CN101664945A (en) * | 2009-07-17 | 2010-03-10 | 中国林业科学研究院木材工业研究所 | Strengthening and flame-retardant modified artificial forest wood and preparation method thereof |
| CN101745951A (en) * | 2009-12-22 | 2010-06-23 | 中国林业科学研究院木材工业研究所 | Modified planted forest timber and preparation method thereof |
| CN102535244A (en) * | 2011-12-23 | 2012-07-04 | 青岛众和恒业蜂窝纸板制品有限公司 | Waterproof flame-retardant honeycomb paper board production process |
| CN103739804A (en) * | 2013-12-25 | 2014-04-23 | 重庆建峰浩康化工有限公司 | Scavenger for free formaldehyde in etherified amino resin and using method thereof |
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2014
- 2014-10-16 CN CN201410549137.2A patent/CN104927012B/en not_active Expired - Fee Related
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1583815A (en) * | 2004-06-11 | 2005-02-23 | 中国化工建设总公司常州涂料化工研究院 | Preparing method for water soluble urea resin |
| WO2006121352A1 (en) * | 2005-05-11 | 2006-11-16 | Fibre 7 Limited | Wood hardening procedures |
| CN101664945A (en) * | 2009-07-17 | 2010-03-10 | 中国林业科学研究院木材工业研究所 | Strengthening and flame-retardant modified artificial forest wood and preparation method thereof |
| CN101745951A (en) * | 2009-12-22 | 2010-06-23 | 中国林业科学研究院木材工业研究所 | Modified planted forest timber and preparation method thereof |
| CN102535244A (en) * | 2011-12-23 | 2012-07-04 | 青岛众和恒业蜂窝纸板制品有限公司 | Waterproof flame-retardant honeycomb paper board production process |
| CN103739804A (en) * | 2013-12-25 | 2014-04-23 | 重庆建峰浩康化工有限公司 | Scavenger for free formaldehyde in etherified amino resin and using method thereof |
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Address after: 578101 Hainan province Lingao County town of dovin Honghua state farm Patentee after: Hainan Long Tai Tai Wood Technology Co., Ltd. Address before: 578101 Hainan province Danzhou Yangpu Economic Development Zone, Jin Yang Lu Pu Xin Wan 19-12-3 Patentee before: YANGPUJIU JUTAI WOOD TECHNOLOGY CO., LTD. |
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Granted publication date: 20170111 Termination date: 20191016 |