CN1101342A - Preparation of N,N,N',N',-tetraacetyl-3,5,3',5'-tetrabromo(chloro)-4,4'-diaminodiphenyl methane - Google Patents
Preparation of N,N,N',N',-tetraacetyl-3,5,3',5'-tetrabromo(chloro)-4,4'-diaminodiphenyl methane Download PDFInfo
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- CN1101342A CN1101342A CN 93118435 CN93118435A CN1101342A CN 1101342 A CN1101342 A CN 1101342A CN 93118435 CN93118435 CN 93118435 CN 93118435 A CN93118435 A CN 93118435A CN 1101342 A CN1101342 A CN 1101342A
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- tetrabromo
- diaminodiphenyl
- methane
- chlorine
- acetylated
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Abstract
The process for preparing 3,5,3'5,-tetraacetyl-3,5,3',5',-tetrabromo (chloro)-4,4'-diaminodiphenyl methane from 3,5,3',5'-tetrabromo (chloro)-4,4'-diaminodiphenyl methane and acetic oxide includes such steps as proportioning, reacting at 105-140 deg.C for 10-60 min., cooling, filter and drying. The product features high purity (over 98.5%) and low cost.
Description
The invention belongs to a kind of with 3,5,3 ', 5 '-tetrabromo (chlorine)-4,4 '-diaminodiphenyl-methane, aceticanhydride are feedstock production N, N, N ', N '-tetra-acetylated-3,5,3 ', 5 '-method of tetrabromo (chlorine)-4,4 ' diaminodiphenyl-methane.
Known N, N, N '; N '-tetra-acetylated-3,5,3 '; 5 '-tetrabromo (chlorine)-4,4 '-to open clear 56-39056 be with 3,5 for the preparation method of diaminodiphenyl-methane such as Japanese Patent spy; 3 ', 5 '-tetrabromo-4,4 '-diaminodiphenyl-methane, aceticanhydride are raw material; dimethylbenzene is solvent; in crystallization-filtration in reaction-immersion water under high pressure, the high temperature, and crude product, Yong diox
Recrystallization gets elaboration.Adopt the aforesaid method weak point to be that facility investment is big, the high, diox of energy consumption price is expensive and to be not easy to obtain, the cost height, residual dimethylbenzene is difficult to clean in the product, and wastewater flow rate is big and be difficult to improvement, has caused environmental pollution.
The invention provides a kind of autoclave that do not adopt is reactor; dimethylbenzene, diox is that solvent prepares N, N, N ', N '-tetra-acetylated-3; 5; 3 '; 5 '-method of tetrabromo (chlorine)-4,4 ' diaminodiphenyl-methane, realize reducing facility investment; do not produce poisonous waste water, improve product purity and be purpose of the present invention.
Realize that the method that purpose of the present invention is taked is with 3,5,3 '; 5 '-tetrabromo (chlorine)-4,4 '-diaminodiphenyl-methane, aceticanhydride is a raw material; join successively to open in the reactor that has stirring and reflux exchanger and stir; intensification was reacted 10～60 minutes under 105～140 ℃ condition, through cooling-filtration-filter cake through alkali cleaning, washing-oven dry-De N, N, N ', N '-tetra-acetylated-3; 5; 3 ', 5 '-tetrabromo (chlorine)-4,4 '-diaminodiphenyl-methane.
Reaction formula is as follows:
Proportioning raw materials (mol ratio):
Aceticanhydride: 3,5,3 ', 5 '-tetrabromo (chlorine)-4,4 '-diaminodiphenyl-methane=15～20: 1
Advantage of the present invention and positively effect:
Adopt method of the present invention to prepare N; N; N ', N '-tetra-acetylated-3,5; 3 '; 5 '-tetrabromo (chlorine)-4,4 ' diaminodiphenyl-methane, facility investment is few; synthesis under normal pressure danger is little, and raw material is based on our country, easily manufacturing, non-environmental-pollution, product purity height (content can reach more than 98.5%).
Embodiment (one)
With 540.6 the gram 3,5,3 '; 5 '-tetrabromo-4; 4 '-aceticanhydrides of diaminodiphenyl-methane and 2081.6 grams join one have stir and the there-necked flask of reflux exchanger in, open stirring, be warming up to 135 ± 2 ℃; insulation reaction is 15 ± 1 minutes under this temperature; then be cooled to room temperature, reaction solution extracted out filtered, filter cake washes with the sodium hydroxide lye of 0.5N; be washed till the washing fluid pH value and be at 8 o'clock and end; use distilled water flushing twice again, washing fluid gets 526ml, gets N after the filter cake drying; N; N ', N '-tetra-acetylated-3,5; 3 '; 5 '-tetrabromo-4,4 '-diaminodiphenyl-methane 579.4 grams, content 98.7%; mother liquor gets 2025 grams; mother liquor 2025 gram put in the matrass distill, the fraction that intercept 115～118 ℃ reclaims acetic acid 634.5 grams, and the fraction recovery aceticanhydride 1388.2 that intercept 140～142 ℃ restrains; washing lotion 526ml also distills, and reclaims acetate and gets sodium-acetate 21g.
Embodiment (two)
With 353.6 the gram 3,5,3 '; 5 '-tetrachloro-4,4 '-diaminodiphenyl-methane and 2081.6 gram aceticanhydrides join one have stir and the there-necked flask of reflux exchanger in, the same embodiment of manufacture craft (); get N, N, N '; N '-tetra-acetylated-3; 5,3 ', 5 '-tetrachloro-4; 4 '-diaminodiphenyl-methane 428.1 grams, content 98.6%.
Claims (2)
1; a kind of with 3,5,3 '; 5 '-tetrabromo (chlorine)-4,4 '-diaminodiphenyl-methane; aceticanhydride is feedstock production N, N; N ', N '-tetra-acetylated-3,5; 3 ', 5 '-method of tetrabromo (chlorine)-4,4 ' diaminodiphenyl-methane; it is characterized in that: with 3,5,3 '; 5 '-tetrabromo (chlorine)-4,4 '-diaminodiphenyl-methane; aceticanhydride joins in the reactor that has stirring and reflux exchanger successively, opens to stir to heat up; under 105～140 ℃ condition, reacted 10～60 minutes, through cooling-filtration-filter cake through alkali cleaning; washing-oven dry-De N; N, N ', N '-tetra-acetylated-3; 5,3 ', 5 '-tetrabromo (chlorine)-4; 4 '-diaminodiphenyl-methane
Proportioning raw materials (mol ratio): aceticanhydride: 3,5,3 ', 5 '-tetrabromo (chlorine)-4,4 '-diaminodiphenyl-methane=15～20: 1.
2, by the described N of claim 1, N, N '; N '-tetra-acetylated-3,5,3 '; 5 '-tetrabromo (chlorine)-4,4 '-preparation method of diaminodiphenyl-methane, it is characterized in that: processing condition can be 135 ± 2 ℃ of temperature; insulation reaction 15 ± 1 minutes then is cooled to room temperature, reaction solution is extracted out filtered; filter cake washes with the sodium hydroxide lye of 0.5N; be washed till the washing fluid pH value and be at 8 o'clock and end, use distilled water flushing twice again, dry finished product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 93118435 CN1101342A (en) | 1993-10-05 | 1993-10-05 | Preparation of N,N,N',N',-tetraacetyl-3,5,3',5'-tetrabromo(chloro)-4,4'-diaminodiphenyl methane |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 93118435 CN1101342A (en) | 1993-10-05 | 1993-10-05 | Preparation of N,N,N',N',-tetraacetyl-3,5,3',5'-tetrabromo(chloro)-4,4'-diaminodiphenyl methane |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1101342A true CN1101342A (en) | 1995-04-12 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 93118435 Pending CN1101342A (en) | 1993-10-05 | 1993-10-05 | Preparation of N,N,N',N',-tetraacetyl-3,5,3',5'-tetrabromo(chloro)-4,4'-diaminodiphenyl methane |
Country Status (1)
| Country | Link |
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| CN (1) | CN1101342A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102604091A (en) * | 2012-01-13 | 2012-07-25 | 东华大学 | Polyimide containing benzimidazole unit and preparation method thereof |
-
1993
- 1993-10-05 CN CN 93118435 patent/CN1101342A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102604091A (en) * | 2012-01-13 | 2012-07-25 | 东华大学 | Polyimide containing benzimidazole unit and preparation method thereof |
| CN102604091B (en) * | 2012-01-13 | 2014-07-02 | 东华大学 | Polyimide containing benzimidazole unit and preparation method thereof |
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| SE01 | Entry into force of request for substantive examination | ||
| C01 | Deemed withdrawal of patent application (patent law 1993) | ||
| WD01 | Invention patent application deemed withdrawn after publication |