CN112851553A - Low-temperature polyurethane cross-linking agent DI-DMA and preparation method thereof - Google Patents
Low-temperature polyurethane cross-linking agent DI-DMA and preparation method thereof Download PDFInfo
- Publication number
- CN112851553A CN112851553A CN202110123003.4A CN202110123003A CN112851553A CN 112851553 A CN112851553 A CN 112851553A CN 202110123003 A CN202110123003 A CN 202110123003A CN 112851553 A CN112851553 A CN 112851553A
- Authority
- CN
- China
- Prior art keywords
- temperature
- linking agent
- dma
- low
- polyurethane cross
- 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.)
- Pending
Links
- 229920002635 polyurethane Polymers 0.000 title claims abstract description 29
- 239000004814 polyurethane Substances 0.000 title claims abstract description 29
- 239000003431 cross linking reagent Substances 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- ROSDSFDQCJNGOL-UHFFFAOYSA-N Dimethylamine Chemical compound CNC ROSDSFDQCJNGOL-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000000843 powder Substances 0.000 claims abstract description 8
- 239000002904 solvent Substances 0.000 claims abstract description 8
- DOETVZCFKJCYJV-UHFFFAOYSA-N 6-(4,5-dihydro-1h-imidazol-2-yl)-2-[4-(4,5-dihydro-1h-imidazol-2-yl)phenyl]-1h-indole Chemical compound N1CCN=C1C1=CC=C(C=2NC3=CC(=CC=C3C=2)C=2NCCN=2)C=C1 DOETVZCFKJCYJV-UHFFFAOYSA-N 0.000 claims abstract description 6
- 101100286286 Dictyostelium discoideum ipi gene Proteins 0.000 claims abstract description 6
- 239000007864 aqueous solution Substances 0.000 claims abstract description 5
- 238000010438 heat treatment Methods 0.000 claims abstract description 5
- 239000003054 catalyst Substances 0.000 claims abstract description 4
- 238000005086 pumping Methods 0.000 claims abstract description 4
- 239000007787 solid Substances 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims abstract description 3
- 125000002147 dimethylamino group Chemical group [H]C([H])([H])N(*)C([H])([H])[H] 0.000 claims description 4
- 239000000853 adhesive Substances 0.000 abstract description 7
- 230000001070 adhesive effect Effects 0.000 abstract description 7
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 2
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 2
- 239000001257 hydrogen Substances 0.000 abstract description 2
- IQPQWNKOIGAROB-UHFFFAOYSA-N isocyanate group Chemical group [N-]=C=O IQPQWNKOIGAROB-UHFFFAOYSA-N 0.000 abstract description 2
- 239000000203 mixture Substances 0.000 abstract description 2
- 229920001187 thermosetting polymer Polymers 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract 1
- 238000004064 recycling Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229920003002 synthetic resin Polymers 0.000 description 1
- 239000000057 synthetic resin Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C275/00—Derivatives of urea, i.e. compounds containing any of the groups, the nitrogen atoms not being part of nitro or nitroso groups
- C07C275/28—Derivatives of urea, i.e. compounds containing any of the groups, the nitrogen atoms not being part of nitro or nitroso groups having nitrogen atoms of urea groups bound to carbon atoms of six-membered aromatic rings of a carbon skeleton
-
- 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
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
-
- 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
- C09J175/00—Adhesives based on polyureas or polyurethanes; Adhesives based on derivatives of such polymers
- C09J175/04—Polyurethanes
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Polyurethanes Or Polyureas (AREA)
Abstract
The invention relates to the technical field of cross-linking agents, and particularly discloses a low-temperature polyurethane cross-linking agent DI-DMA and a preparation method thereof, wherein the low-temperature polyurethane cross-linking agent DI-DMA is white powder; the manufacturing method comprises the following steps: adding a solvent into a reaction kettle, and adding a catalyst; pumping DIPI into a reaction kettle at room temperature, heating, gradually dropwise adding a dimethylamine aqueous solution, controlling the reaction temperature at 80-90 ℃, keeping the temperature for 4 hours, starting desolventizing, recovering and recycling the solvent, and then starting centrifuging to obtain solid white powder. The low-temperature polyurethane cross-linking agent DI-DMA and the preparation method thereof have simple process, the prepared low-temperature polyurethane cross-linking agent DI-DMA is a single-component thermosetting low-temperature polyurethane cross-linking agent, active hydrogen or isocyanate groups in the composition exist in a closed form, and the single-component polyurethane adhesive cured by a heat source has good stability, good adhesive strength and heat resistance.
Description
Technical Field
The invention belongs to the technical field of cross-linking agents, and particularly relates to a low-temperature polyurethane cross-linking agent DI-DMA and a preparation method thereof.
Background
Polyurethane, known as polyurethane, is a versatile synthetic resin with a variety of product forms. The polyurethane cross-linking agent DI-DMA is mainly applied to polyurethane adhesives, and can be divided into single components and double components according to the chemical properties and the packaging form of the polyurethane adhesives due to various types of the polyurethane cross-linking agent DI-DMA.
Disclosure of Invention
The invention aims to provide a low-temperature polyurethane cross-linking agent DI-DMA and a preparation method thereof, and a polyurethane adhesive with good stability and good bonding strength is prepared.
In order to solve the technical problem, the invention provides a low-temperature polyurethane crosslinking agent DI-DMA, which is white powder and has the following structural general formula:
the invention also provides a preparation method of the low-temperature polyurethane cross-linking agent DI-DMA, which is characterized by comprising the following specific steps:
s1, adding a solvent into the reaction kettle, and adding a catalyst;
s2, pumping DIPI into a reaction kettle at room temperature, heating and raising the temperature, gradually dropwise adding a dimethylamine aqueous solution, controlling the reaction temperature at 80-90 ℃, and preserving the temperature for 4 hours;
and S3, starting desolventizing, recovering the solvent, and then starting centrifuging to obtain solid white powder.
Further, when the aqueous dimethylamine solution is added into the S2, the reaction is carried out, and the dimethylamine residue is controlled to be not higher than 2% of the end of the reaction.
The invention has the beneficial effects that: the low-temperature polyurethane cross-linking agent DI-DMA and the preparation method thereof have simple process, the prepared low-temperature polyurethane cross-linking agent DI-DMA is a single-component thermosetting low-temperature polyurethane cross-linking agent, active hydrogen or isocyanate groups in the composition exist in a closed form, and the single-component polyurethane adhesive cured by a heat source has good stability, good adhesive strength and heat resistance.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In one embodiment of the present invention, specifically disclosed is a low temperature polyurethane crosslinking agent DI-DMA, which is a white powder having the following general structural formula:
the invention also discloses a preparation method of the low-temperature polyurethane cross-linking agent DI-DMA, which is characterized by comprising the following specific steps:
s1, adding a DIPI solvent into the reaction kettle, and adding a catalyst for reaction;
s2, pumping the reacted DIPI into a reaction kettle at room temperature, heating and raising the temperature, gradually dripping dimethylamine aqueous solution for reaction, controlling the reaction temperature to be 80-90 degrees, and keeping the temperature for 4 hours when the reaction is finished and the dimethylamine residue is not higher than 2 percent;
and S3, starting desolventizing, recovering the solvent, and then starting centrifuging to obtain solid white powder.
The above disclosure is only one preferred embodiment of the present invention, and certainly should not be construed as limiting the scope of the invention, which is defined by the claims and their equivalents.
Claims (3)
1. A low temperature polyurethane cross-linking agent DI-DMA is characterized in that the low temperature polyurethane cross-linking agent DI-DMA is white powder and has the following structural general formula:
2. a preparation method of a low-temperature polyurethane cross-linking agent DI-DMA is characterized by comprising the following specific steps:
s1, adding a DIPI solvent into the reaction kettle, and adding a catalyst for reaction;
s2, pumping the reacted DIPI into a reaction kettle at room temperature, heating and heating, gradually dropwise adding a dimethylamine aqueous solution, controlling the reaction temperature to be 80-90 ℃, and keeping the temperature for 4 hours when the reaction is finished and the dimethylamine residue is not higher than 2%;
and S3, starting desolventizing, recovering the solvent, and then starting centrifuging to obtain solid white powder.
3. The method for preparing DI-DMA of low temperature polyurethane cross-linking agent as claimed in claim 1, wherein the reaction of adding dimethylamine aqueous solution dropwise into S2 is controlled to control dimethylamine residue not higher than 2% at the end of the reaction.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110123003.4A CN112851553A (en) | 2021-01-29 | 2021-01-29 | Low-temperature polyurethane cross-linking agent DI-DMA and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110123003.4A CN112851553A (en) | 2021-01-29 | 2021-01-29 | Low-temperature polyurethane cross-linking agent DI-DMA and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN112851553A true CN112851553A (en) | 2021-05-28 |
Family
ID=75986658
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110123003.4A Pending CN112851553A (en) | 2021-01-29 | 2021-01-29 | Low-temperature polyurethane cross-linking agent DI-DMA and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112851553A (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3956237A (en) * | 1974-07-08 | 1976-05-11 | The Dow Chemical Company | Epoxy resin compositions comprising latent amine curing agents and novel accelerators |
| US4387105A (en) * | 1982-01-26 | 1983-06-07 | American Cyanamid Company | Methods of treating atherosclerosis with dialkylureas and dialkylthioureas |
| CN102432599A (en) * | 2011-10-31 | 2012-05-02 | 成都地奥制药集团有限公司 | Crystal form of oxalate of dipeptidyl peptidase inhibitor and preparation method and application thereof |
| CN112119107A (en) * | 2018-05-17 | 2020-12-22 | 赫克塞尔合成有限公司 | Improved curing agent composition |
-
2021
- 2021-01-29 CN CN202110123003.4A patent/CN112851553A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3956237A (en) * | 1974-07-08 | 1976-05-11 | The Dow Chemical Company | Epoxy resin compositions comprising latent amine curing agents and novel accelerators |
| US4387105A (en) * | 1982-01-26 | 1983-06-07 | American Cyanamid Company | Methods of treating atherosclerosis with dialkylureas and dialkylthioureas |
| CN102432599A (en) * | 2011-10-31 | 2012-05-02 | 成都地奥制药集团有限公司 | Crystal form of oxalate of dipeptidyl peptidase inhibitor and preparation method and application thereof |
| CN112119107A (en) * | 2018-05-17 | 2020-12-22 | 赫克塞尔合成有限公司 | Improved curing agent composition |
Non-Patent Citations (2)
| Title |
|---|
| DEVRIES, VERN G.等: ""Potential antiatherosclerotic agents. 6. Hypocholesterolemic trisubstituted urea analogs"", 《JOURNAL OF MEDICINAL CHEMISTRY》 * |
| 李俊贤: "《塑料工业手册 聚氨酯》", 30 July 1999, 化学工业出版社 * |
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| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20210528 |