CN100443417C - Recovery method for waste water of 1,4-dihydroxyanthraquinone production - Google Patents
Recovery method for waste water of 1,4-dihydroxyanthraquinone production Download PDFInfo
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- CN100443417C CN100443417C CNB200410013484XA CN200410013484A CN100443417C CN 100443417 C CN100443417 C CN 100443417C CN B200410013484X A CNB200410013484X A CN B200410013484XA CN 200410013484 A CN200410013484 A CN 200410013484A CN 100443417 C CN100443417 C CN 100443417C
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- dihydroxyanthraquinone
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Abstract
The present invention discloses a recovery method for process waste water of 1, 4-dihydroxyanthraquinone, which comprises the processes of concentration, cooling, crystallization, separation and drying. The 1, 4-dihydroxyanthraquinone process waste water is processed by condensation till the sulfuric acid concentration is from 20% to 80%, and then, the process waste water is cooled to 30 to 0 DEG C for crystallization; crystallization pulp material is processed by liquid solid separation, a filtering body is sulfuric acid with the concentration of 20 to 80%, and a filter cake is dried to obtain compounds containing phthalic acid, boric acid and 2-hydroxyl-5-chlorine-6'-carboxyl benzophenone.
Description
Technical field
The present invention relates to a kind of 1, the recovery method of 4-dihydroxyanthraquinone processing wastewater, particularly a kind of recovery 1, phthalic acid in the 4-dihydroxyanthraquinone processing wastewater, boric acid, 2-hydroxyl-5-chloro-6 '-mixture and the vitriolic method of carboxyl benzophenone.
Background technology
1,4-dihydroxyanthraquinone processing wastewater has two kinds of treatment processs at present: the one, and waste water is through neutralizing, coagulate treatment process such as wadding, biochemistry, decolouring; The 2nd, waste water is after low temperature crystallization reclaims phthalic acid, again through treatment process such as neutralization, flocculation, biochemistry, decolourings.Aforesaid method waste water reclamation rate is low, needs a large amount of alkali neutralizations, the processing costs height, and be difficult to qualified discharge, cause the bigger wasting of resources and environmental pollution.
Summary of the invention
Purpose of the present invention will provide a kind of 1 exactly, the recovery method of 4-dihydroxyanthraquinone processing wastewater, its adopt to concentrate, cooling, crystallization, separation and exsiccant technological process, can solve existing 1,4-dihydroxyanthraquinone waste water treatment recovery technology weak effect causes the wasting of resources and environmental pollution problems.
The object of the present invention is achieved like this: a kind of 1, the recovery method of 4-dihydroxyanthraquinone processing wastewater comprises concentrated, cooling, crystallization, separation and drying process, and concrete steps are:
A. concentrate: with 1, the waste water that 4-dihydroxyanthraquinone technology produces is concentrated into the solution that sulfur acid concentration is 20%-80%,
B. cooling: it is 30 ℃-0 ℃ that the solution after will concentrating is cooled to temperature with tap water or refrigerated water,
C. crystallization: keeping concentrated solution is 30 ℃-0 ℃ in temperature, under nature or whipped state, and phthalic acid wherein, boric acid, 2-hydroxyl-5-chloro-6 '-mixed crystallization of carboxyl benzophenone separates out,
D. separate: will have the crystalline slurry and carry out liquid-solid separation, filter cake be phthalic acid, boric acid, 2-hydroxyl-5-chloro-6 '-mixture of carboxyl benzophenone, filtrate is that concentration is the sulfuric acid of 20%-80%,
E. dry: is under 100 ℃-110 ℃ with isolated filter cake in the D step in normal pressure, temperature, is dried to moisture content less than 0.5%.
Adopt the inventive method, recyclable 1, phthalic acid in the 4-dihydroxyanthraquinone processing wastewater, boric acid, 2-hydroxyl-5-chloro-6 '-chemical substance such as carboxyl benzophenone and sulfuric acid, to produce 1000 grams 1, the processing wastewater meter of 4-dihydroxyanthraquinone product, recyclable sulfuric acid 3400 grams (rolling over 100% sulphur acid meter) wherein, phthalic acid, boric acid, 2-hydroxyl-5-chloro-6 '-carboxyl benzophenone mixture 500 grams, compare with conventional art, can economize on resources, reduce by 1 greatly, 4-dihydroxyanthraquinone production cost has also been stopped industrial wastewater pollution simultaneously.
Description of drawings
Below in conjunction with drawings and Examples the present invention is further described.
Fig. 1 is a process flow diagram of the present invention.
Embodiment
As shown in Figure 1, quantitatively with 1,4-dihydroxyanthraquinone processing wastewater adds in the thickener, and being heated to the continuous evaporation concentration of boiling point to solution sulfur acid concentration is 20%-80%, stops heating; Rapidly concentrated solution is put into cooling crystallizer again, chuck, coil pipe or tubulation water flowing cooling, and open and stir, wait to expect temperature drop to 30 ℃-0 ℃ after, stay on more than one hour, wherein phthalic acid, boric acid, 2-hydroxyl-5-chloro-6 '-crystalline mixture of carboxyl benzophenone separates out.Then slurry is carried out liquid-solid separation with separating device.Filtrate is that concentration is the sulfuric acid of 20%-80%, and filter cake is put into moisture eliminator, temperature be 100 ℃-110 ℃ down dry, until moisture content less than 0.5%, get final product phthalic acid, boric acid, 2-hydroxyl-5-chloro-6 '-mixture of carboxyl benzophenone.
The inventive method also can be used for 1,4-dihydroxyanthraquinone and derived product thereof or derivative (as: 1,4-diamino-anthraquinone leuco compound, 99%1,4-dihydroxyanthraquinone etc.) phthalic acid in the processing wastewater that preceding operation 1,4-dihydroxyanthraquinone are produced, boric acid, 2-hydroxyl-5-chloro-6 '-mixture and the vitriolic of carboxyl benzophenone reclaim.
To produce 50 grams 1, the waste water 1750ml that the 4-dihydroxyanthraquinone produces is that example illustrates technological process of the present invention below.
Embodiment one:
1750ml waste water is added in the 2000ml beaker, and add several in zeolite, Sheng liquid beaker is placed on to be heated on the 1KW electric furnace and boils, evaporation concentration is during to solution sulfur acid concentration 20%, stop heating, the beaker that to contain concentrated solution is then put into water-bath and is cooled off, and constantly stir with glass stick, treat that material is cooled to 30 ℃, have mass crystallization to separate out, stayed on one hour, then this slurry is filtered on B, get 20% sulphuric acid soln 800ml, filter cake in 100 ℃ of-110 ℃ of oven dry, gets phthalic acid in CLS101-E type baking oven, boric acid, 2-hydroxyl-5-chloro-6 '-the mixture 25g of carboxyl benzophenone.
Embodiment two:
1750ml waste water is added in the 2000ml beaker, and add several in zeolite, Sheng liquid beaker is placed on to be heated on the 1KW electric furnace and boils, evaporation concentration is during to solution sulfur acid concentration 30%, stop heating, the beaker that to contain concentrated solution is then put into water-bath and is cooled off, and constantly stir with glass stick, treat that material is cooled to below 15 ℃, have mass crystallization to separate out, stayed on one hour, this slurry is filtered on B, get 30% sulphuric acid soln 570ml, filter cake in 100 ℃ of-110 ℃ of oven dry, gets phthalic acid in CLS101-E type baking oven, boric acid, 2-hydroxyl-5-chloro-6 '-the mixture 31g of carboxyl benzophenone.
Claims (1)
1, a kind of 1, the recovery method of 4-dihydroxyanthraquinone processing wastewater comprises concentrated, cooling, crystallization, separation and drying process, it is characterized in that:
A. concentrate: with 1, the waste water that 4-dihydroxyanthraquinone technology produces is concentrated into the solution that sulfur acid concentration is 20%-80%,
B. cooling: it is 30 ℃-0 ℃ that the solution after will concentrating is cooled to temperature with tap water or refrigerated water,
C. crystallization: keeping concentrated solution is 30 ℃-0 ℃ in temperature, under nature or whipped state, and phthalic acid wherein, boric acid, 2-hydroxyl-5-chloro-6 '-mixed crystallization of carboxyl benzophenone separates out,
D. separate: will have the crystalline slurry and carry out liquid-solid separation, filter cake be phthalic acid, boric acid, 2-hydroxyl-5-chloro-6 '-mixture of carboxyl benzophenone, filtrate is that concentration is the sulfuric acid of 20%-80%,
E. dry: is under 100 ℃-110 ℃ with isolated filter cake in the D step in normal pressure, temperature, is dried to moisture content less than 0.5%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB200410013484XA CN100443417C (en) | 2004-07-16 | 2004-07-16 | Recovery method for waste water of 1,4-dihydroxyanthraquinone production |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB200410013484XA CN100443417C (en) | 2004-07-16 | 2004-07-16 | Recovery method for waste water of 1,4-dihydroxyanthraquinone production |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1594111A CN1594111A (en) | 2005-03-16 |
| CN100443417C true CN100443417C (en) | 2008-12-17 |
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| Application Number | Title | Priority Date | Filing Date |
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| CNB200410013484XA Expired - Fee Related CN100443417C (en) | 2004-07-16 | 2004-07-16 | Recovery method for waste water of 1,4-dihydroxyanthraquinone production |
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104445781B (en) * | 2014-11-27 | 2016-03-23 | 浙江奇彩环境科技股份有限公司 | A kind of administering method of fused ring compound waste water |
| CN114988630B (en) * | 2022-06-29 | 2023-05-09 | 甘肃金缘泰新材料有限公司 | Method and system for recycling waste sulfuric acid containing boric acid by using 1, 4-dihydroxyanthraquinone |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3810833A (en) * | 1971-09-02 | 1974-05-14 | North Western Gas Board | Purification processes |
| CN1280102A (en) * | 2000-07-10 | 2001-01-17 | 南京大学 | Treatment and source recovering method for waste water of 1,4-dihydroxy anthraquinone produetion |
| CN1288883A (en) * | 1999-09-16 | 2001-03-28 | 游川北 | Low-temperature crystallization process to recover phthalic acid from chemical waste water |
-
2004
- 2004-07-16 CN CNB200410013484XA patent/CN100443417C/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3810833A (en) * | 1971-09-02 | 1974-05-14 | North Western Gas Board | Purification processes |
| CN1288883A (en) * | 1999-09-16 | 2001-03-28 | 游川北 | Low-temperature crystallization process to recover phthalic acid from chemical waste water |
| CN1280102A (en) * | 2000-07-10 | 2001-01-17 | 南京大学 | Treatment and source recovering method for waste water of 1,4-dihydroxy anthraquinone produetion |
Non-Patent Citations (4)
| Title |
|---|
| 1,4－二羟基蒽醌废水处理工艺设计. 徐淦和，张善发.上海冶金专科学校学报，第16卷第4期. 1995 |
| 1,4－二羟基蒽醌废水处理工艺设计. 徐淦和，张善发.上海冶金专科学校学报，第16卷第4期. 1995 * |
| 树脂吸附法处理1,4－二羟基蒽醌生产废水的研究. 张晓，张全兴，陈金龙.离子交换与吸附，第16卷第2期. 2000 |
| 树脂吸附法处理1,4－二羟基蒽醌生产废水的研究. 张晓，张全兴，陈金龙.离子交换与吸附，第16卷第2期. 2000 * |
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| CN1594111A (en) | 2005-03-16 |
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Granted publication date: 20081217 Termination date: 20170716 |