CN112812712A - Flame-retardant adhesive and application thereof - Google Patents
Flame-retardant adhesive and application thereof Download PDFInfo
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- CN112812712A CN112812712A CN202110214722.7A CN202110214722A CN112812712A CN 112812712 A CN112812712 A CN 112812712A CN 202110214722 A CN202110214722 A CN 202110214722A CN 112812712 A CN112812712 A CN 112812712A
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- 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
- C09J129/00—Adhesives based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Adhesives based on hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Adhesives based on derivatives of such polymers
- C09J129/02—Homopolymers or copolymers of unsaturated alcohols
- C09J129/04—Polyvinyl alcohol; Partially hydrolysed homopolymers or copolymers of esters of unsaturated alcohols with saturated carboxylic acids
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- 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
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention discloses a flame-retardant adhesive and application thereof, wherein a main agent polyvinyl alcohol in an aqueous polymer-isocyanate adhesive is subjected to phosphorylation modification, a phosphorus-silicon flame retardant is used as a filler of the aqueous polymer-isocyanate adhesive to prepare the adhesive with flame-retardant property, and the prepared flame-retardant adhesive is applied to a single board to be glued, assembled and hot-pressed according to a conventional process to prepare the flame-retardant plywood. The preparation method provided by the invention is simple and suitable for large-scale popularization.
Description
Technical Field
The invention relates to the field of artificial board processing, in particular to a flame-retardant adhesive and application thereof.
Background
The plywood is one of common materials for furniture and interior decoration, and is one of three artificial boards. Along with the improvement of people to quality of life and the attention degree of self physical and mental health promotes gradually, highly attach attention to the free formaldehyde that releases in the plywood, it is not looked at to the healthy negative impact who causes of people. The aqueous polymer-isocyanate adhesive is used as a formaldehyde-release-free adhesive and is more and more widely applied, but the aqueous polymer-isocyanate adhesive has no flame retardant property, and although the plywood prepared by using the aqueous polymer-isocyanate adhesive has no formaldehyde release, the prepared plywood has poor flame retardant property and has larger potential safety hazard in use; if a flame retardant is added into the aqueous polymer-isocyanate adhesive, the main agent (polyvinyl alcohol) of the aqueous polymer-isocyanate adhesive is generally poor in compatibility with the flame retardant, and the stable adhesive is difficult to prepare by combining the main agent and the flame retardant. Therefore, the preparation of an adhesive which does not release formaldehyde and has flame retardant property is a technical problem to be solved in the field.
Disclosure of Invention
The invention aims to provide a flame-retardant adhesive and application thereof, and aims to solve the problem that an aldehyde-free adhesive does not have flame-retardant performance; meanwhile, the prepared flame-retardant adhesive is applied to the preparation of plywood to prepare the plywood with flame-retardant performance.
In order to achieve the purpose, the invention provides the following technical scheme:
one of the technical schemes of the invention is as follows: the flame-retardant adhesive is prepared by taking polyvinyl alcohol phosphate and an ethylene-vinyl acetate copolymer as main agents and taking a phosphorus-silicon flame retardant as a filler.
Preferably, the flame retardant is prepared by taking polyvinyl alcohol phosphate and ethylene-vinyl acetate copolymer as main agents, poly diphenylmethane diisocyanate (P-MDI) as a curing agent and phosphorus silicon flame retardant as a filler.
Preferably, the mass ratio of the polyvinyl alcohol phosphate to the ethylene-vinyl acetate copolymer is 7: 3; the dosage of the P-MDI is 10 percent of the mass of the main agent; the using amount of the phosphorus-silicon flame retardant is 30 percent of the mass of the main agent.
When the phosphorus-silicon flame retardant is used for flame retardance, the generated carbon layer can be more compact due to the silicon element, and the carbon layer can be promoted to generate metaphosphoric acid due to the phosphorus element, so that a phosphorus-silicon synergistic effect is generated, and the flame retardance efficiency is improved.
Preferably, the preparation method of the polyvinyl alcohol phosphate comprises the following steps: mixing polyvinyl alcohol and phosphoric acid, heating to 50 ℃, adding urea, continuously heating to 95 ℃, adding the phosphoric acid solution again, reacting for 3 hours, cooling to normal temperature after the reaction is finished, precipitating with ethanol, washing the precipitate, and drying to obtain the polyvinyl alcohol phosphate.
The synthesis reaction equation of the polyvinyl alcohol phosphate is as follows:
the phosphate-esterified polyvinyl alcohol can destroy hydroxyl groups regularly arranged in the polyvinyl alcohol, so that the acting force between molecules is reduced, the mixed solution is more stable by taking the polyvinyl alcohol phosphate as a main agent, the compatibility among all elements is increased, and a certain flame retardant effect is provided for the aqueous polymer-isocyanate adhesive on the basis of the above.
According to the invention, the reaction temperature and the phosphoric acid dosage are changed to carry out esterification reaction on the main agent polyvinyl alcohol in the aqueous polymer-isocyanate adhesive, so as to prepare the polyvinyl alcohol phosphate (PPVA). During the thermal decomposition of phosphoric acid molecules in the polyvinyl alcohol phosphate, moisture is generated, the condensation temperature is further reduced, and the combustible gas is diluted to ensure that the overall concentration is reduced.
Preferably, the phosphoric acid is 85% phosphoric acid, wherein the mass volume ratio of the polyvinyl alcohol to the urea to the phosphoric acid is 10g to 20g (16.25-16.35) ml, the first adding amount of the phosphoric acid is 16ml, and the second adding amount of the phosphoric acid is 0.25-0.35 ml.
Preferably, the washing solution used for washing is absolute ethyl alcohol, and the pH value is 5-6.
Preferably, the phosphorus-silicon flame retardant is a DOPO-POSS flame retardant.
The 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO) contains a biphenyl ring and a phenanthrene ring structure, so that the DOPO shows a plurality of excellent performances, and simultaneously has a hypophosphite structure, a P-C bond exists in a molecule, the hydrolysis resistance is good, the DOPO has good thermal stability and chemical stability, the activity of the P-H bond in the DOPO is very high, and the DOPO can react with functional groups such as an unsaturated bond, a carbonyl group, an epoxy group and the like, and can be used as a reactive flame retardant to participate in the reaction and also can be used as an additive flame retardant to retard a high polymer material; the polyhedral oligomeric silsesquioxane (POSS) molecules limit the movement of polymer molecules, so that the thermal stability is improved, and the DOPO-POSS condensate formed by the polyhedral oligomeric silsesquioxane (POSS) molecules has excellent flame retardant property. DOPO-POSS is used as a filler of the aqueous polymer-isocyanate adhesive, so that a certain flame retardant effect can be provided for the aqueous polymer-isocyanate adhesive; the DOPO-POSS can also participate in the cross-linking reaction of the water-based polymer and the polyisocyanate, and the DOPO-POSS molecules are cured into a cross-linked net structure of the water-based polymer and the polyisocyanate, so that the phenomenon of plate moisture absorption and the defect of flame retardant migration caused by adding the DOPO-POSS flame retardant are improved, and the permanent flame retardant effect is achieved.
Preferably, the preparation method of the DOPO-POSS flame retardant comprises the following steps: mixing DOPO and VTES, stirring uniformly, adding Azobisisobutyronitrile (AIBN), heating to 80-85 ℃, continuing stirring, and reacting for 10-12h to obtain triethoxysilane (DOPO-VTES); dissolving the prepared DOPO-VTES in a methanol solution, heating to 80-85 ℃, adding hydrochloric acid, condensing, refluxing, stirring, and reacting for 24-26 h; and separating the reaction liquid, washing the upper layer solution with toluene, filtering, combining the filter residue with the lower layer solution, concentrating and drying to obtain the DOPO-POSS flame retardant.
More preferably, in the process of preparing DOPO-VTES, the molar ratio of DOPO, VTES and AIBN is 1 (2-6) to (2-5); the stirring speed in the mixing process is 450 r/min; adding AIBN, and stirring at 550 r/min; the temperature is raised to 81 ℃; the reaction time is 10 h;
in the process of preparing the DOPO-POSS flame retardant, the mass-volume ratio of DOPO-VTES, methanol and hydrochloric acid is (10-12) g:50ml:3.2 ml; the stirring speed is 600 r/min; the temperature was raised to 81 ℃ and the reaction time was 24 h.
The second technical scheme of the invention is as follows: the application of the flame-retardant adhesive in the flame-retardant plywood is provided.
Preferably, the flame-retardant adhesive is applied with glue on a single board according to a conventional process, and then assembled and hot-pressed to obtain the flame-retardant plywood.
Preferably, the veneer is a poplar veneer with the water content of 10-12% and the tree age of 5-6 years; the glue coating amount of the flame-retardant adhesive on the veneer is 120-300g/m2。
The invention has the following beneficial technical effects:
according to the invention, the main agent polyvinyl alcohol in the aqueous polymer-isocyanate adhesive is modified by phosphorylation, and the phosphorus-silicon flame retardant is used as the filler of the aqueous polymer-isocyanate adhesive to prepare the adhesive with flame retardant property. The preparation method provided by the invention is simple and suitable for large-scale popularization.
Drawings
FIG. 1 is an infrared spectrum of polyvinyl alcohol and polyvinyl alcohol phosphate prepared in example 1.
Detailed Description
Reference will now be made in detail to various exemplary embodiments of the present invention, examples of which are illustrated in the accompanying drawings, and this detailed description should not be taken to be limiting of the invention, but is rather a more detailed description of certain aspects, features and embodiments of the invention. It is to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
Further, for numerical ranges in this disclosure, it is understood that each intervening value, between the upper and lower limit of that range, is also specifically disclosed. Every smaller range between any stated value or intervening value in a stated range and any other stated or intervening value in a stated range is encompassed within the invention. The upper and lower limits of these smaller ranges may independently be included or excluded in the range.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Although only preferred methods and materials are described herein, any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention.
As used herein, the terms "comprising," "including," "having," "containing," and the like are open-ended terms that mean including, but not limited to.
Example 1
Preparation of flame-retardant plywood containing DOPO-POSS flame retardant
(1) Preparation of DOPO-POSS flame retardant
10.0938g DOPO and 10g VTES are added into a 100ml three-neck flask with a magnetic stirring device, and then stirring is started continuously, and the stirring speed is adjusted to 450 r/min; 0.1665g of AIBN is added after uniform stirring, the mixture is heated in an oil bath and slowly heated to 81 ℃, the stirring speed is adjusted to 550r/min, the reaction lasts for 10 hours, the substances in the flask become clear and have pungent odor, and DOPO-VTES is prepared, the yield is 16.9g, and the yield is 83%.
Dissolving 10.1g of DOPO-VTES in 50ml of methanol solution in a 100ml three-neck flask with a magnetic stirring device and a condensation reflux device, heating in an oil bath, slowly heating to 81 ℃, then slowly dropwise adding 3.2ml of hydrochloric acid solution into the three-neck flask, adjusting the stirring speed to 600r/min, and reacting for 24 hours; after the reaction is finished, separating the reaction liquid, taking the upper layer solution, washing the upper layer solution with toluene, filtering, combining the filter residue and the lower layer solution, concentrating until a viscous substance is formed, putting the viscous substance into an oven to dry for 6 hours at the drying temperature of 70 ℃ to prepare the DOPO-POSS flame retardant with the yield of 3.4938g and the yield of 35%.
(2) Preparation of polyvinyl alcohol phosphate
10g of polyvinyl alcohol and 16ml of 85 percent phosphoric acid are put into a 500ml three-neck flask for heating and stirring reaction; when the temperature of the solution reaches 50 ℃, adding 20g of urea as a catalyst, and then heating to 95 ℃ to completely dissolve the polyvinyl alcohol; continuously dropwise adding 0.35ml of 85% phosphoric acid, and reacting for 3h at 95 ℃; after the reaction is finished, cooling the solution to normal temperature, and then precipitating the obtained polyvinyl alcohol phosphate by using absolute ethyl alcohol. Shearing the precipitate, washing with anhydrous ethanol until the pH value is stabilized at 5-6; and (3) putting the mixture into a vacuum drying oven, and drying the mixture in vacuum at the temperature of 50 ℃ to constant weight to obtain the polyvinyl alcohol phosphate.
(3) Preparation of flame-retardant adhesive
And (2) preparing a flame-retardant adhesive with the solid content of 56% and the viscosity of 100 Mpa.s by using 70g of the polyvinyl alcohol phosphate prepared in the step (2) and 30g of the ethylene-vinyl acetate copolymer as main agents, 10g of P-MDI as a curing agent and 30g of the DOPO-POSS flame retardant prepared in the step (1) as a filler.
(4) Pressing of flame-retardant plywood
The producing area is northern China, the age of the tree is 5-6 years, the water content is 10% -12%, the size is 300mm multiplied by 3mm, and the density is 0.85g/cm3The poplar is a veneer, the flame-retardant adhesive prepared in the step (3) is coated according to a conventional process, and the glue application amount is 120g/m2Paving the mixed material, performing prepressing treatment, performing penetrating steam preheating and hot pressing, and performing hot press molding to prepare the flame-retardant plywood; the hot pressing temperature is 110 ℃, the time is 180s, and the pressure is 2.5 MPa.
Example 2
Compared with example 1, the difference is that the addition amount of the filler is 20g, and the sizing amount is 200g/m2The other steps and parameters were the same as in example 1.
Example 3
Compared with example 1, the difference is that the adding amount of the filler is 40g, and the sizing amount is 300g/m2The other steps and parameters were the same as in example 1.
Example 4
Compared with example 1, the difference is that the addition amount of the filler is 50g, and the sizing amount is 220g/m2The other steps and parameters were the same as in example 1.
Example 5
Compared with example 1, the difference is that the adding amount of the filler is 60g, and the sizing amount is 180g/m2The other steps and parameters were the same as in example 1.
Example 6
Compared with example 1, the difference is that the addition amount of the filler is 70g, and the sizing amount is 150g/m2The other steps and parameters were the same as in example 1.
Comparative example 1
Compared with example 1, the step (1) is omitted, CaCO is selected3The procedure and parameters were the same as in example 1, except that DOPO-POSS flame retardant was replaced as a filler.
Comparative example 2
Compared with the embodiment 1, the step (2) is omitted, 70g of polyvinyl alcohol and 30g of ethylene-vinyl acetate copolymer are selected as main agents, and other steps and parameters are the same as the embodiment 1.
FIG. 1 is an infrared spectrum of polyvinyl alcohol and polyvinyl alcohol phosphate prepared in example 1. As can be seen by comparing the infrared spectrum of PVA with that of PPVA in FIG. 1, the infrared spectrum of PPVA is 1697cm higher than that of PVA-1Left and right-C ═ O-disappearance (1379 cm)-1Absorption peaks of medium-strength-P ═ O-bonds appear on the left and the right, which indicates that phosphate is introduced into hydroxyl on one side of PVA to carry out esterification reaction, and phosphate groups are formed, wherein the absorption peak of medium-strength is the coincidence of the absorption peak of-P-O-C and the absorption peak of lipid C-O stretching vibration. And is at 1697cm-1The strong absorption peak shows that the esterification reaction really occurs by combining the absorption peaks of-P ═ O-and-P-O-C and showing that-P-O-C and-P ═ O-are present.
The bonding strength of the flame-retardant plywood prepared in the examples 1-6 and the comparative examples 1-2 is detected according to GB/T17657 and 2013 physicochemical property test method for artificial boards and decorative artificial boards; the impact strength of the flame-retardant plywood prepared in examples 1-6 and comparative examples 1-2 was tested according to GB/T9846-; part 2 of the combustion behaviour was determined according to GB/T2406.2-2009 "oxygen index for plastics: room temperature test the oxygen index of the flame retardant plywood prepared in examples 1-6 and comparative examples 1-2 was measured, and the results are shown in Table 1:
TABLE 1 measurement results of Properties of flame retardant plywood prepared in examples 1-6 and comparative examples 1-2
As can be seen from Table 1, example 1 is the best formulation disclosed in the present invention, and all the effects are good. The flame retardant property of the board prepared in the embodiments 1-6 of the invention can meet the B-grade or C-grade building fire-proof grade, and the physical and mechanical properties can reach the national standard.
The above-described embodiments are merely illustrative of the preferred embodiments of the present invention, and do not limit the scope of the present invention, and various modifications and improvements of the technical solutions of the present invention can be made by those skilled in the art without departing from the spirit of the present invention, and the technical solutions of the present invention are within the scope of the present invention defined by the claims.
Claims (10)
1. The flame-retardant adhesive is characterized by being prepared by taking polyvinyl alcohol phosphate and an ethylene-vinyl acetate copolymer as main agents and a phosphorus-silicon flame retardant as a filler.
2. The flame-retardant adhesive of claim 1, wherein the flame-retardant adhesive is prepared by taking polyvinyl alcohol phosphate and an ethylene-vinyl acetate copolymer as main agents, P-MDI as a curing agent and a phosphorus-silicon flame retardant as a filler.
3. The flame retardant adhesive of claim 2, wherein the mass ratio of the polyvinyl alcohol phosphate to the ethylene-vinyl acetate copolymer is 7: 3; the dosage of the P-MDI is 10 percent of the mass of the main agent; the using amount of the phosphorus-silicon flame retardant is 20-70% of the mass of the main agent.
4. The flame-retardant adhesive according to claim 1, wherein the preparation method of the polyvinyl alcohol phosphate comprises the following steps: mixing polyvinyl alcohol and phosphoric acid, heating to 50 ℃, adding urea, continuously heating to 95 ℃, adding phosphoric acid again, reacting for 3 hours, cooling to normal temperature after the reaction is finished, precipitating with ethanol, washing the precipitate, and drying to obtain the polyvinyl alcohol phosphate.
5. The flame-retardant adhesive as claimed in claim 4, wherein the phosphoric acid is 85% phosphoric acid, the mass volume ratio of the polyvinyl alcohol to the urea to the phosphoric acid is 10g to 20g (16.25-16.35) ml, the first addition amount of the phosphoric acid is 16ml, and the second addition amount of the phosphoric acid is 0.25-0.35 ml.
6. The flame retardant adhesive of claim 1 wherein the phosphorus silicon flame retardant is a DOPO-POSS flame retardant; the preparation method of the DOPO-POSS flame retardant comprises the following steps: mixing DOPO and VTES, stirring uniformly, adding AIBN, heating to 80-85 ℃, continuing stirring, and reacting for 10-12h to obtain DOPO-VTES; dissolving the prepared DOPO-VTES in methanol, heating to 80-85 ℃, adding hydrochloric acid, condensing, refluxing, stirring, and reacting for 24-30 h; and separating the reaction liquid, washing the upper layer solution with toluene, filtering, combining the filter residue with the lower layer solution, concentrating and drying to obtain the DOPO-POSS flame retardant.
7. The flame retardant adhesive of claim 6 wherein the molar ratio of DOPO, VTES and AIBN during the preparation of DOPO-VTES is 1 (2-6) to (2-5); the stirring speed in the mixing process is 450 r/min; adding AIBN, and stirring at 550 r/min;
in the process of preparing the DOPO-POSS flame retardant, the mass-volume ratio of DOPO-VTES, methanol and hydrochloric acid is (10-12) g:50ml:3.2 ml; the stirring speed was 600 r/min.
8. Use of the flame retardant adhesive of any one of claims 1-7 in the preparation of flame retardant plywood.
9. The application of the flame-retardant adhesive in the flame-retardant plywood is characterized in that the flame-retardant adhesive is coated on single boards, assembled and hot-pressed to obtain the flame-retardant plywood.
10. The application of claim 9, wherein the veneer is a poplar veneer with a water content of 10% -12% and a tree age of 5-6 years; the glue coating amount of the flame-retardant adhesive on the veneer is 120-300g/m2。
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113858376A (en) * | 2021-09-27 | 2021-12-31 | 湖南九富家居材料有限公司 | Preparation method of high-strength environment-friendly ecological plate |
| CN116144296A (en) * | 2023-01-06 | 2023-05-23 | 银川七彩涂饰有限公司 | Low-temperature-resistant zero-formaldehyde water-based adhesive and preparation process thereof |
| CN117363298A (en) * | 2023-10-09 | 2024-01-09 | 江西欣美新材料科技有限公司 | Halogen-free flame-retardant functional polyurethane sealant and preparation process thereof |
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| WO2016095289A1 (en) * | 2014-12-17 | 2016-06-23 | 杨磊 | Preparation method for nanometer material capable of improving fire resistance of waterborne polyurethane coating and adhesive |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113858376A (en) * | 2021-09-27 | 2021-12-31 | 湖南九富家居材料有限公司 | Preparation method of high-strength environment-friendly ecological plate |
| CN116144296A (en) * | 2023-01-06 | 2023-05-23 | 银川七彩涂饰有限公司 | Low-temperature-resistant zero-formaldehyde water-based adhesive and preparation process thereof |
| CN116144296B (en) * | 2023-01-06 | 2023-11-10 | 银川七彩涂饰有限公司 | Low-temperature-resistant zero-formaldehyde water-based adhesive and preparation process thereof |
| CN117363298A (en) * | 2023-10-09 | 2024-01-09 | 江西欣美新材料科技有限公司 | Halogen-free flame-retardant functional polyurethane sealant and preparation process thereof |
| CN117363298B (en) * | 2023-10-09 | 2024-05-07 | 江西欣美新材料科技有限公司 | Halogen-free flame-retardant functional polyurethane sealant and preparation process thereof |
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| CN112812712B (en) | 2022-06-03 |
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