CN101962431A - Urushiol phosphorous-series flame retardant resin and preparation method thereof - Google Patents
Urushiol phosphorous-series flame retardant resin and preparation method thereof Download PDFInfo
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- CN101962431A CN101962431A CN 201010506602 CN201010506602A CN101962431A CN 101962431 A CN101962431 A CN 101962431A CN 201010506602 CN201010506602 CN 201010506602 CN 201010506602 A CN201010506602 A CN 201010506602A CN 101962431 A CN101962431 A CN 101962431A
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- laccol
- retardant resin
- phosphorous
- phosphorous flame
- urushiol
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Abstract
The invention discloses urushiol phosphorous-series flame retardant resin. The resin consists of the following raw materials in percentage by mass: 20 to 40 percent of urushiol, 0 to 20 percent of amine compound, 4 to 10 percent of aldehyde compound, 0.5 to 6 percent of phosphorous-series compound, 0 to 5 percent of epoxy resin, 0.5 to 3 percent of catalyst and 40 to 55 percent of solvent. A method for preparing the urushiol phosphorous-series flame retardant resin comprises the following steps of: obtaining raw lacquer from a lacquer tree; separating and extracting the urushiol from the raw lacquer, heating the urushiol and reacting the heated urushiol with the amine compound, the aldehyde compound, the solvent and the catalyst for synthesizing; and adding the epoxy resin, the phosphorous-series compound and the solvent into the complex, heating and reacting for synthesizing, stopping heating and cooling to room temperature after reaction is finished. The resin has high flame retardant property, water resistance and chemical resistance and is suitable for fields such as public fire safety, chemical industry, light industry, building materials, electronic apparatuses, mining and the like.
Description
Technical field
The present invention relates to a kind of anti-flaming dope, particularly a kind of laccol phosphorous flame-retardant resin and preparation thereof are mainly used in fields such as public fire protection safety, chemical industry, light industry, weaving, building materials, electronic apparatus, mining.
Background technology
China's raw lacquer aboundresources, the various coating varieties that utilize raw lacquer to make are various, along with rapid development of social economy, people require day by day to raise for the flame retardant properties of coating, every field is for the also variation more of demand of anti-flaming dope, the use of novel flame redundant material in the national economy field meets the indication of central authorities about " preventing trouble before it happens ", it is the prerequisite of guaranteeing people's life, national resources safety, than fire protection preventive means more one step ahead, domestic and international market is mathematical to the novel flame-retardant product demand.But existing anti-flaming dope fails to keep the excellent properties of raw lacquer mostly, can not overcome the sensitization problem of raw lacquer, also has certain limitation in the use.Therefore, utilize advantageous raw lacquer resource of China and performance advantage, on the basis that keeps the raw lacquer excellent properties,, synthesize laccol anti-flaming dope and have very important significance with good flame-retardance energy according to the response characteristic of laccol in the raw lacquer.
Summary of the invention
The objective of the invention is to, on the basis that keeps the raw lacquer premium properties, provide a kind of laccol phosphorous flame-retardant resin and preparation thereof, to overcome raw lacquer or cashew resin material limitation in the use.The present invention according to the response characteristic of laccol in the raw lacquer, utilizes itself and phosphorus series compound to react and the laccol phosphorous flame-retardant resin that obtains having flame retardant properties on the basis that keeps the raw lacquer excellent properties.
In order to realize above-mentioned task, the present invention adopts following technical solution:
A kind of laccol phosphorous flame-retardant resin, this laccol phosphorous flame-retardant resin that makes is made up of following raw materials according and mass percent thereof: laccol: 20%～40%, aminated compounds: 0～20%, aldehyde compound: 4%～10%, phosphorus series compound: 0.5%～6%, Resins, epoxy: 0%～5%, catalyzer: 0.5%～3%, solvent: 40%～55%, the per-cent sum of above-mentioned raw materials is 100%.
Described laccol is that Qi, city mouth Qi, hair dam Qi, Qin Ling Qi or other areas produce extraction in the lacquer from peace health Qi, the Chinese, fries in shallow oil the dish mark more than 65%, and laccol content is more than 50%.
Described aminated compounds is aniline, in aniline, adjacent aniline or the triethylamine one or more.
Described aldehyde compound is one or more in formaldehyde, furfural or the polyoxymethylene.
Described phosphorus series compound is one or more in phosphorus oxide, phosphorus oxychloride, the phosphoric acid fat.
Described solvent is one or more in dimethylbenzene, butanols or the pimelinketone.
The preparation method of above-mentioned laccol phosphorous flame-retardant resin comprises the steps:
Step 1, method routinely is the separation and Extraction laccol from raw lacquer, obtains laccol solution behind the solvent of adding formula ratio, the aminated compounds, aldehyde compound and the catalyzer that in laccol solution, add formula ratio, be heated to 60～100 ℃, reacted 2～6 hours, dehydration heats up;
Step 2 treats that system temperature rises to 90～145 ℃, adds the Resins, epoxy and the phosphoric acid ester of formula ratio in the material that obtains, and reacts 1～5 hour, stops to reduce to room temperature after the heating, promptly gets laccol phosphorous flame-retardant resin.
Laccol phosphorous flame-retardant resin of the present invention has overcome the sensitization problem of raw lacquer, can spray, can be coated with, can brush, and is not high to construction technical requirement, and can realize mechanized, do not need specific temperature and humidity condition, can be dry under field conditions (factors), paint film has kept the premium properties of raw lacquer.Have excellent flame-retardant, acidproof, water-fast, medium-resistance is good.
The present invention is described in further detail below in conjunction with embodiment.
Embodiment
The laccol phosphorous flame-retardant resin that the present invention makes is made up of following raw materials according and mass percent thereof: laccol: 20%～40%, aminated compounds: 0～20%, aldehyde compound: 4%～10%, phosphorus series compound: 0.5%～6%, Resins, epoxy: 0%～5%, catalyzer: 0.5%～3%, solvent: 40%～55%, the per-cent sum of above-mentioned raw materials is 100%.
The preparation method of above-mentioned laccol phosphorous flame-retardant resin comprises: method routinely is the separation and Extraction laccol from raw lacquer, obtain laccol solution after adding the solvent of formula ratio then, the aminated compounds, aldehyde compound and the catalyzer that in laccol solution, add formula ratio again, be heated to 60～100 ℃, reacted 2～6 hours, and heated up and slough the small molecules product water; In the material that obtains, add the Resins, epoxy and the phosphorus series compound of formula ratio, be heated to 90～145 ℃, reacted 1～4 hour, stop to reduce to room temperature after the heating, promptly get laccol phosphorous flame-retardant resin.
Described laccol is that Qi, city mouth Qi, hair dam Qi, Qin Ling Qi or other areas produce extraction in the lacquer from peace health Qi, the Chinese, fries in shallow oil the dish mark more than 65%, and laccol content is more than 50%.
Described phosphorus series compound is one or more in phosphorus oxide, phosphorus oxychloride, the phosphoric acid fat.
Described aminated compounds is aniline, in aniline, adjacent aniline or the triethylamine one or more.
Described aldehyde compound is one or more in formaldehyde, furfural or the polyoxymethylene.
Described solvent is one or more in dimethylbenzene, butanols or the pimelinketone.
Embodiment 1:
The weight percent of laccol phosphorous flame-retardant resin raw material of the present invention is as follows:
Described laccol is that Qi, city mouth Qi, hair dam Qi, Qin Ling Qi or other areas produce in the lacquer routinely method extraction from peace health Qi, the Chinese, fries in shallow oil and coils mark more than 65%, and laccol content is more than 50%.
The dimethylbenzene that the laccol that extracts in the raw lacquer is added formula ratio, obtain laccol solution, laccol solution is heated to 60 ℃, the formaldehyde, the ammoniacal liquor that add formula ratio reacted 1-3 hour, and the dehydration that heats up treats that system temperature rises to 110 ℃, the phosphoric acid ester that adds formula ratio, reaction 1-3 hour, reaction is reduced to room temperature after finishing, and promptly gets laccol phosphorous flame-retardant resin.
Embodiment 2:
The raw material and the weight percent of laccol phosphorous flame-retardant resin of the present invention are as follows:
Described laccol be from peace health Qi, the Chinese Qi, city mouth Qi, hair dam Qi, Qin Ling Qi or other areas produces coat with lacquer in routinely method extraction.
The dimethylbenzene that the laccol that extracts in the raw lacquer is added formula ratio obtains laccol solution, laccol solution is heated to 60 ℃, the aniline, furfural and the sodium hydroxide that add formula ratio reacted 2-5 hour, dehydration heats up, treat that system temperature rises to 90 ℃, add the phosphorus oxide of formula ratio, reacted 2-4 hour, reaction finishes to reduce to room temperature, promptly gets laccol phosphorous flame-retardant resin.
Embodiment 3:
The raw material and the weight percent of laccol phosphorous flame-retardant resin of the present invention are as follows:
Described laccol be from peace health Qi, the Chinese Qi, city mouth Qi, hair dam Qi, Qin Ling Qi or other areas produces coat with lacquer in routinely method extraction.
The dimethylbenzene that the laccol that extracts in the raw lacquer is added formula ratio obtains laccol solution, laccol solution is heated to 70 ℃, add formaldehyde, potassium hydroxide reaction 2-5 hour, dehydration heats up, treat system temperature to 110 ℃, add the phosphorus oxychloride and the Resins, epoxy of formula ratio, reacted 3-5 hour, reaction is reduced to room temperature after finishing, and promptly gets laccol phosphorous flame-retardant resin.
Embodiment 4:
The raw material and the weight percent of laccol phosphorous flame-retardant resin of the present invention are as follows:
Described laccol is that Qi, city mouth Qi, hair dam Qi, Qin Ling Qi or other areas produce to coat with lacquer and squeeze in a conventional manner or lixiviate forms from peace health Qi, the Chinese.Fry in shallow oil the dish mark more than 65%, laccol content is more than 50%.
The dimethylbenzene that the laccol that extracts in the raw lacquer is added formula ratio obtains laccol solution, laccol solution is heated to 100 ℃, add formaldehyde, ammoniacal liquor reaction 2-3 hour, heat up, treat that system temperature rises to 145 ℃, add the phosphorus oxychloride and the Resins, epoxy of formula ratio, reacted 2-3 hour, reaction is reduced to room temperature after finishing, and promptly gets laccol phosphorous flame-retardant resin.
The foregoing description is wherein preferable example just, the invention is not restricted to these embodiment, as long as in the formula range that the present invention provides, all can make the laccol phosphorous flame-retardant resin of excellent property.
The present invention uses according to general coating using method, and the spontaneous curing of brushing back is dry to get final product, and dried hardness of paint film height is water-fast, chemical resistance is strong, especially has excellent heat resisting.
The technical feature of the laccol phosphorous flame-retardant resin of the present invention's preparation sees Table 1.
Table 1 laccol phosphorous flame-retardant resin property index
As can be seen from Table 1, the laccol phosphorous flame-retardant resin of the present invention preparation has excellent flame-retardant, and is acidproof, water-fast, medium-resistance is good.
Claims (6)
1. laccol phosphorous flame-retardant resin, it is characterized in that, this laccol phosphorous flame-retardant resin that makes is made up of following raw materials according and mass percent thereof: laccol: 20%～40%, aminated compounds: 0～20%, aldehyde compound: 4%～10%, phosphorus series compound: 0.5%～6%, Resins, epoxy: 0%～5%, catalyzer: 0.5%～3%, solvent: 40%～55%, the per-cent sum of above-mentioned raw materials is 100%.
2. laccol phosphorous flame-retardant resin as claimed in claim 1, it is characterized in that, described laccol is that Qi, city mouth Qi, hair dam Qi, Qin Ling Qi or other areas produce extraction in the lacquer from peace health Qi, the Chinese, fries in shallow oil the dish mark more than 65%, and laccol content is more than 50%.
3. laccol phosphorous flame-retardant resin as claimed in claim 1 is characterized in that, described aminated compounds is aniline, in aniline, adjacent aniline or the triethylamine one or more.
4. laccol phosphorous flame-retardant resin as claimed in claim 1 is characterized in that described aldehyde compound is one or more in formaldehyde, furfural or the polyoxymethylene.
5. laccol phosphorous flame-retardant resin as claimed in claim 1 is characterized in that described solvent is one or more in dimethylbenzene, butanols or the pimelinketone.
6. the preparation method of the described laccol phosphorous flame-retardant of claim 1 resin is characterized in that, comprises the steps:
Step 1, method routinely is the separation and Extraction laccol from raw lacquer, obtains laccol solution behind the solvent of adding formula ratio, the aminated compounds, aldehyde compound and the catalyzer that in laccol solution, add formula ratio, be heated to 60～100 ℃, reacted 2～6 hours, dehydration heats up;
Step 2 treats that system temperature rises to 90～145 ℃, adds the Resins, epoxy and the phosphoric acid ester of formula ratio in the material that obtains, reacting by heating 1～5 hour, and reaction is reduced to room temperature after finishing, and promptly gets laccol phosphorous flame-retardant resin.
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| Application Number | Priority Date | Filing Date | Title |
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| CN 201010506602 CN101962431B (en) | 2010-10-14 | 2010-10-14 | Urushiol phosphorous-series flame retardant resin and preparation method thereof |
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| CN 201010506602 CN101962431B (en) | 2010-10-14 | 2010-10-14 | Urushiol phosphorous-series flame retardant resin and preparation method thereof |
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| CN101962431A true CN101962431A (en) | 2011-02-02 |
| CN101962431B CN101962431B (en) | 2013-04-03 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103044666A (en) * | 2012-12-17 | 2013-04-17 | 中华全国供销合作总社西安生漆涂料研究所 | Synthetic method of urushiol biology base resin |
| CN109880568A (en) * | 2019-03-04 | 2019-06-14 | 闽江学院 | Fire retardant pressure sensitive glue and its application |
| CN109897217A (en) * | 2019-03-04 | 2019-06-18 | 闽江学院 | Double carboxyl-functional laccol base phosphonium flame retardants and its preparation method and application |
| CN109929098A (en) * | 2019-03-04 | 2019-06-25 | 闽江学院 | A kind of polymer and preparation method thereof and laccol base phosphor-containing flame-proof pressure sensitive adhesive |
| CN110408319A (en) * | 2019-08-20 | 2019-11-05 | 闽江学院 | Fire-retardant raw lacquer film and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1115328A (en) * | 1994-03-25 | 1996-01-24 | 武汉大学 | Self-drying urushiol furol varnish |
| CN101302399A (en) * | 2008-06-20 | 2008-11-12 | 中华全国供销合作总社西安生漆涂料研究所 | Urushiol screen print coating |
-
2010
- 2010-10-14 CN CN 201010506602 patent/CN101962431B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1115328A (en) * | 1994-03-25 | 1996-01-24 | 武汉大学 | Self-drying urushiol furol varnish |
| CN101302399A (en) * | 2008-06-20 | 2008-11-12 | 中华全国供销合作总社西安生漆涂料研究所 | Urushiol screen print coating |
Non-Patent Citations (1)
| Title |
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| 《阻燃材料与技术》 19981231 贾伟华等 耐热、阻燃酚醛树脂的合成 正文2.2耐热、阻燃酚醛树脂的合成 1-6 , 第2期 2 * |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103044666A (en) * | 2012-12-17 | 2013-04-17 | 中华全国供销合作总社西安生漆涂料研究所 | Synthetic method of urushiol biology base resin |
| CN109880568A (en) * | 2019-03-04 | 2019-06-14 | 闽江学院 | Fire retardant pressure sensitive glue and its application |
| CN109897217A (en) * | 2019-03-04 | 2019-06-18 | 闽江学院 | Double carboxyl-functional laccol base phosphonium flame retardants and its preparation method and application |
| CN109929098A (en) * | 2019-03-04 | 2019-06-25 | 闽江学院 | A kind of polymer and preparation method thereof and laccol base phosphor-containing flame-proof pressure sensitive adhesive |
| CN109897217B (en) * | 2019-03-04 | 2021-01-26 | 闽江学院 | Double-carboxyl functional urushiol-based phosphorus-containing flame retardant and preparation method and application thereof |
| CN109929098B (en) * | 2019-03-04 | 2021-03-02 | 闽江学院 | Polymer, preparation method thereof and urushiol-based phosphorus-containing flame-retardant pressure-sensitive adhesive |
| CN109880568B (en) * | 2019-03-04 | 2021-05-25 | 闽江学院 | Flame-retardant pressure-sensitive adhesive and application thereof |
| CN110408319A (en) * | 2019-08-20 | 2019-11-05 | 闽江学院 | Fire-retardant raw lacquer film and preparation method thereof |
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| CN101962431B (en) | 2013-04-03 |
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