CN1036337C - Method for production of pentamethyl-divinyl-triamine catalyst during production of polyurethane soft foamed plastics - Google Patents

Method for production of pentamethyl-divinyl-triamine catalyst during production of polyurethane soft foamed plastics Download PDF

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Publication number
CN1036337C
CN1036337C CN93110707A CN93110707A CN1036337C CN 1036337 C CN1036337 C CN 1036337C CN 93110707 A CN93110707 A CN 93110707A CN 93110707 A CN93110707 A CN 93110707A CN 1036337 C CN1036337 C CN 1036337C
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Prior art keywords
production
hour
heated
methyl diethylentriamine
foamed plastics
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Expired - Fee Related
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CN93110707A
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CN1093699A (en
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纪文富
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JINTAN CITY ASSISTANTS FACTORY
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JINTAN CITY ASSISTANTS FACTORY
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/08—Processes
    • C08G18/16—Catalysts
    • C08G18/18—Catalysts containing secondary or tertiary amines or salts thereof
    • C08G18/1808—Catalysts containing secondary or tertiary amines or salts thereof having alkylene polyamine groups
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G2110/00—Foam properties
    • C08G2110/0008—Foam properties flexible

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The present invention relates to a catalyst in chemical production, particularly to a production method for a pentamethyldiethylenetriamine catalyst in the production of flexible foam plastics made from polyurethane. Chemical raw material, such as formic acid, formaldehyde, etc., which can be easily obtained are processed by the following steps of stirring, dropping, heating, dewatering, etc. to carry out a chemical reaction thoroughly, so that the pentamethyldiethylenetriamine catalyst is obtained. Compared with abroad production methods, the method of the present invention has the advantages of simple and practical process, easy obtainment of the raw materials, little investment, short production periodicity, low cost, good quality, no three waste products, etc.

Description

The production method of five methyl diethylentriamine catalyzer during polyurethane soft foamed plastics is produced
The present invention relates to the catalyzer in a kind of Chemical Manufacture, the production method of the five methyl diethylentriamine catalyzer in particularly a kind of polyurethane flexible plastics-production.
Now, in polyurethane soft foamed plastics is produced, mostly adopt triethylenediamine to make catalyzer, it is not high that its shortcoming not only makes the quality of polyurethane soft foamed plastics carry, and in process of production, its processing quality is uncontrollable, causes proportioning to be difficult to grasp, the product physicals is poor, also has a large amount of three wastes handling problem etc.At present, some enterprise adopts the five methyl diethylentriamine of import to make catalyzer, but will spend a large amount of foreign exchanges aborning, and the cost height, and the limited amount of import holds up work for lack of material often.There is three wastes problem in external production method complexity, the cost height of producing this catalyzer, and is not suitable for China's national situation.
Purpose of the present invention is exactly at above-mentioned defective and deficiency, develops a kind of new production method of five methyl diethylentriamine catalyzer of suitable China's national situation, to address the above problem.
Technical scheme of the present invention:
1, drops into raw material formic acid, formaldehyde to reactor, be warming up to 60-90 ℃, stir;
2, slowly drip diethylenetriamine, dripped time 2-5 hour;
3, be warming up to 100-120 ℃ again, fully (backflow) reaction, time 3-8 hour;
HCOOH+HCHO+(NH 2CH 2CH 2) 2NH—→
Figure C9311070700031
4, be cooled to 100 ℃, dehydration;
5, add an amount of sodium hydroxide, draw moisture content;
6, leave standstill 3-9 hour, reduce to normal temperature, remove the water and the sodium hydroxide raffinate of lower floor, get thick product;
7, thick product is dropped in the still kettle, be heated to 100 ℃, slough remaining moisture content again;
8, continue to be heated to 105-125 ℃, separate low-boiling amine;
9, continue to be heated to 160-180 ℃ again, the five methyl diethylentriamine vaporization receives by condensing works, promptly gets smart product five methyl diethylentriamine.
That the method that the invention has the advantages that the external relatively producer of its method has is simple and practical, investment is little, the cycle short, raw material is easy to get, easy to operate in the production process, nothing three waste products, advantages such as the product cost of producing is low, quality is good, and filled up domestic blank, be import substitute, can be country and save a large amount of foreign exchanges.
Other advantage of the present invention will further be set forth below.
Embodiment:
With content is that 276 kilograms in 85% formic acid and content are that 480 kilograms in 37% formaldehyde drops in the normal-pressure reaction kettle of 1000 liters, and its chemical molecular formula is:
Formic acid HCOOH
Formaldehyde HCHO is warming up to 70-75 ℃, stirs simultaneously; Slowly at the uniform velocity drip content then and be 93 kilograms of 98% diethylenetriamine, its chemical molecular formula is:
Diethylenetriamine (NH 2CH 2CH 2) 2The NH time that drips is grasped by under meter, is controlled in 3-4 hour, dropwises, and is warming up to 110 ℃ again, allow solution fully carry out chemical reaction, and with backflow phenomenon, its chemical equation is:
HCOOH+HCHO+ (NH 2CH 2CH 2) 2NH-→
Figure C9311070700041
Wherein the mole ratio of each stock yard is: formaldehyde: formic acid: diethylenetriamine=6.4: 5.6: 1, and the reaction times was controlled at 5-6 hour; Question response is cooled to 100 ℃ after finishing again, makes the water evaporates vaporization, reaches the dehydration purpose, and dehydrating amount is generally the 30-40% of theoretical water content; Then, add sodium hydroxide, add-on is the 20-25% of total reaction liquid, the moisture content in the draw solution, then with the solution left standstill 5-6 in the reactor hour, temperature is under the normal temperature, and the water and the sodium hydroxide raffinate that will be in lower floor are removed, and get thick product, again thick product is dropped in the still kettle, be heated to 100 ℃, make wherein remaining moisture content carburation by evaporation, continue heat temperature raising to 115 ℃, make the low-boiling amine carburation by evaporation, receive by condenser, stand-by as the raw material of reaction next time, continue to be heated to 177 ℃ again, the five methyl diethylentriamine vaporization, receive by condenser, promptly get 135 kilograms of smart product five methyl diethylentriamines, content is 98%.

Claims (1)

1, the production method of five methyl diethylentriamine catalyzer during polyurethane soft foamed plastics is produced is characterized in that:
(1) raw material formic acid, formaldehyde are dropped in the reactor, be warming up to 60-90 ℃, stir simultaneously;
(2) slowly at the uniform velocity drip diethylenetriamine then, the dropping time is 2-5 hour;
(3) be warming up to 100-120 ℃ again, fully (backflow) reaction, its chemical equation is:
HCOOH+HCHO+ (NH 2CH 2CH 2) 2NH---→ Reaction times 3-8 hour;
(4) be cooled to 100 ℃, dehydration;
(5) add an amount of sodium hydroxide, draw moisture content;
(6) leave standstill 3-9 hour, reduce to normal temperature, remove the water and the sodium hydroxide raffinate of lower floor, get thick product;
(7) thick product is dropped in the still kettle, be heated to 100 ℃, slough remaining moisture content again;
(8) continue to be heated to 105-125 ℃, separate low-boiling amine;
(9) continue to be heated to 160-180 ℃ again, the five methyl diethylentriamine vaporization receives by condensing works, promptly gets smart product five methyl diethylentriamine.
CN93110707A 1993-03-10 1993-03-10 Method for production of pentamethyl-divinyl-triamine catalyst during production of polyurethane soft foamed plastics Expired - Fee Related CN1036337C (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN93110707A CN1036337C (en) 1993-03-10 1993-03-10 Method for production of pentamethyl-divinyl-triamine catalyst during production of polyurethane soft foamed plastics

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Application Number Priority Date Filing Date Title
CN93110707A CN1036337C (en) 1993-03-10 1993-03-10 Method for production of pentamethyl-divinyl-triamine catalyst during production of polyurethane soft foamed plastics

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CN1093699A CN1093699A (en) 1994-10-19
CN1036337C true CN1036337C (en) 1997-11-05

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Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102942493A (en) * 2012-11-09 2013-02-27 西南石油大学 Terquaternary cation surface active agent and preparation method
CN104628602B (en) * 2015-02-05 2016-08-17 宋和璇 Tetramethyl diethylenetriamine base formiate compound and its preparation method and application

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4020059A (en) * 1975-06-02 1977-04-26 Nippon Shokubai Kagaku Kogyo Co., Ltd. Process for preparing tertiary amines

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4020059A (en) * 1975-06-02 1977-04-26 Nippon Shokubai Kagaku Kogyo Co., Ltd. Process for preparing tertiary amines

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
《HELVETICA CH1M1CA,ACTA.》34卷,P23-931页 1951.1.1 *

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