CN102993060B - Preparation method of 1,6-naphthalenedisulfonic acid disodium salt - Google Patents
Preparation method of 1,6-naphthalenedisulfonic acid disodium salt Download PDFInfo
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- CN102993060B CN102993060B CN201210264674.3A CN201210264674A CN102993060B CN 102993060 B CN102993060 B CN 102993060B CN 201210264674 A CN201210264674 A CN 201210264674A CN 102993060 B CN102993060 B CN 102993060B
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Abstract
The invention discloses a preparation method of 1,6-naphthalenedisulfonic acid disodium salt. The 1, 6-naphthalenedisulfonic acid disodium salt is prepared from the following components as raw materials: 77-91 percent of 1,6-naphthalene disulfonic acid, 1-3 percent of 1,5-naphthalene disulfonic acid and 4-11 percent of sulfuric acid. The preparation method comprises the following steps: 1, adding the 1,6-naphthalene disulfonic acid and water to a reactor according to a weight ratio of 2:1 to obtain a mixture; 2, heating the mixture to 40-60 DEG C to dissolve, adjusting the pH value to 2-4 by using a 30% sodium hydroxide solution, wherein the heating temperature is 100-110 DEG C; 3, stopping heating the solution when the crystallization temperature is 30-40 DEG C; 4, cooling to the solution to 20-30 DEG C, and slowing heating to 55-65 DEG C; 5, preserving the temperature and filtering the 1,5-naphthalene disulfonic acid out; and 6, cooling the filtrate to 15-30 DEG C, and centrifuging the cooled solution to the 1,6-naphthalenedisulfonic acid disodium salt. The 1, 6-naphthalenedisulfonic acid disodium salt prepared by using the preparation method disclosed by the invention is high in purity.
Description
Technical field
The invention belongs to chemical field, particularly a kind of 1,6-naphthalene disulfonate preparation method.
Background technology
1,6-naphthalene disulfonate is important dyestuffs industries intermediate, belongs to one of product of " product restructuring guidance list " (basis in 2011) encourage growth.1,6-naphthalene disulfonate, through constant-pressure and high-temperature alkali fusion, can make 1,6-dihydroxy naphthlene.1,6-dihydroxy naphthlene and the coupling of multiple heavy helium component can obtain a series of acid mordant dyes, are mainly used in the industries such as silk, cashmere and wool spinning.Along with the development of industrial and agricultural production and going deep into of every research, its purposes will become more and more extensive.
Current 1,6-naphthalene disulfonate salify technology is: in 1,6-naphthalene disulfonate, add sodium hydroxide salify, obtain 1,6-naphthalene disulfonate through crystallization, after centrifugal.The weak point of prior art is: because 1,5-naphthalene disulfonate solubleness in water is less, in the time of crystallization with 1,6-naphthalene disulfonate is separated out, cause obtaining after centrifugal 1,6-naphthalene disulfonate purity is lower, generally can be higher than 96%, bring a lot of disadvantageous effects to lower step industrial production.
Summary of the invention
For above-mentioned the deficiencies in the prior art, the object of this invention is to provide a kind of product purity high 1,6-naphthalene disulfonate preparation method.
Technical scheme of the present invention is: a kind of 1,6-naphthalene disulfonate preparation method, the raw material 1 using, 6-naphthalene disulfonic acid component is: 1 of 77-91%, 6-naphthalene disulfonic acid, 1 of 1-3%, 5-naphthalene disulfonic acid, the sulfuric acid of 4-11%, above per-cent is mass percent, it is characterized in that: the method comprises following operation steps:
Step 1: in reactor, add raw material 1,6-naphthalene disulfonic acid and water, its Raw 1, the weight ratio of 6-naphthalene disulfonic acid and water is 2: 1;
Step 2: said mixture is warming up to after 40-60 DEG C of dissolving, and being adjusted to pH value with 30% sodium hydroxide solution is 2-4, then heating is concentrated, and Heating temperature is 100-110 DEG C;
Step 3: when the Tc of survey solution is 30-40 DEG C, stop heating;
Step 4: first solution is cooled to 20-30 DEG C, and then be slowly warmed up to 55-75 DEG C;
Step 5: be incubated filtration after completing above-mentioned intensification, filter out 1,5-naphthalene disulfonate;
Step 6: filtrate is cooled to 15-30 DEG C, obtains 1,6-naphthalene disulfonate after centrifugal.
Further, the Tc of solution described in described step 3 is 32-37 DEG C.
Further, the temperature slowly heating up described in described step 4 is 58-62 DEG C.
Further, the excellent 18-25 DEG C of the cooling temperature of filtrate described in described step 5.
Advantageous effect of the present invention is: the present invention is by being controlled to the degree of crystallinity of salts solution, first be down to a specified temp, then after being slowly warmed up to an assigned temperature, insulation is filtered, remove 1,5 naphthalene disulfonates, by cooling filtrate centrifugal, obtain generally more than 99% with this highly purified 1,6-naphthalene disulfonate product.
Embodiment
Below in conjunction with specific embodiment, the invention will be further described, the raw material 1 that various embodiments of the present invention are used, the consisting of of 6-naphthalene disulfonic acid: 1 of 77-91%, 6-naphthalene disulfonic acid, 1 of 1-3%, 5-naphthalene disulfonic acid, the sulfuric acid of 4-11%, also has some other impurity.
Embodiment mono-
A kind of 1,6-naphthalene disulfonate preparation method, comprises following operation steps:
Step 1: in reactor, add 2000kg1,6-naphthalene disulfonic acid and 1000kg water,
Step 2: by said mixture to 40-60 DEG C of dissolving, with the molten pH value that is adjusted to of 30% sodium hydroxide be 2, then heating is concentrated, Heating temperature is 100 DEG C,
Step 3: when the Tc of survey solution is 30 DEG C, stop heating;
Step 4: first solution is cooled to 20 DEG C, and then be slowly warmed up to 55 DEG C;
Step 5: be incubated filtration after completing above-mentioned intensification, filter out 1,5-naphthalene disulfonate;
Step 6: filtrate is cooled to 15 DEG C, obtains 1,6-naphthalene disulfonate 980kg after centrifugal.
Embodiment bis-
A kind of 1,6-naphthalene disulfonate preparation method, comprises following operation steps:
Step 1: in reactor, add 2000kg1,6-naphthalene disulfonic acid and 1000kg water,
Step 2: to 40-60 DEG C of dissolving, being adjusted to pH value with 30% sodium hydroxide solution is 4 by said mixture, then heating is concentrated, and Heating temperature is 100 DEG C,
Step 3: when the Tc of survey solution is 30 DEG C, stop heating;
Step 4: first solution is cooled to 30 DEG C, and then be slowly warmed up to 65 DEG C;
Step 5: be incubated filtration after completing above-mentioned intensification, filter out 1,5-naphthalene disulfonate;
Step 6: filtrate is cooled to 30 DEG C, obtains 1,6-naphthalene disulfonate 1000kg after centrifugal.
Embodiment tri-
A kind of 1,6-naphthalene disulfonate preparation method, comprises following operation steps:
Step 1: in reactor, add 2000kg1,6-naphthalene disulfonic acid and 1000kg water,
Step 2: to 40-60 DEG C of dissolving, being adjusted to pH value with 30% sodium hydroxide solution is 3 by said mixture, then heating is concentrated, and Heating temperature is 105 DEG C,
Step 3: when the Tc of survey solution is 32 DEG C, stop heating;
Step 4: first solution is cooled to 35 DEG C, and then be slowly warmed up to 58 DEG C;
Step 5: be incubated filtration after completing above-mentioned intensification, filter out 1,5-naphthalene disulfonate;
Step 6: filtrate is cooled to 18 DEG C, obtains 1,6-naphthalene disulfonate 1010kg after centrifugal.
Embodiment tetra-
A kind of 1,6-naphthalene disulfonate preparation method, comprises following operation steps:
Step 1: in reactor, add 2000kg1,6-naphthalene disulfonic acid and 1000kg water,
Step 2: to 40-60 DEG C of dissolving, being adjusted to pH value with 30% sodium hydroxide solution is 3 by said mixture, then heating is concentrated, and Heating temperature is 105 DEG C,
Step 3: when the Tc of survey solution is 32 DEG C, stop heating;
Step 4: first solution is cooled to 35 DEG C, and then be slowly warmed up to 58 DEG C;
Step 5: be incubated filtration after completing above-mentioned intensification, filter out 1,5-naphthalene disulfonate;
Step 6: filtrate is cooled to 18 DEG C, obtains 1,6-naphthalene disulfonate solid 990kg after centrifugal, purity is more than 99%.
Embodiment recited above is described the preferred embodiment of the present invention; not the spirit and scope of the present invention are limited; do not departing under the prerequisite of design concept of the present invention; various modification and improvement that in this area, common engineering technical personnel make technical scheme of the present invention, all should fall into protection scope of the present invention.
Claims (4)
1. one kind 1,6-naphthalene disulfonate preparation method, the raw material 1 using, 6-naphthalene disulfonic acid component is: 77-91% 1,6-naphthalene disulfonic acid, 1 of 1-3%, 5-naphthalene disulfonic acid, the sulfuric acid of 4-11%, above per-cent is mass percent, it is characterized in that: the method comprises following operation steps:
Step 1: in reactor, add raw material 1,6-naphthalene disulfonic acid and water, its Raw 1, the weight ratio of 6-naphthalene disulfonic acid and water is 2:1;
Step 2: said mixture is warming up to after 40-60 DEG C of dissolving, and being adjusted to pH value with 30% sodium hydroxide solution is 2-4, then heating is concentrated, and Heating temperature is 100-110 DEG C;
Step 3: when the Tc of survey solution is 30-40 DEG C, stop heating;
Step 4: first solution is cooled to 20-30 DEG C, and then be slowly warmed up to 55-75 DEG C;
Step 5: be incubated filtration after completing above-mentioned intensification, filter out 1,5-naphthalene disulfonate;
Step 6: filtrate is cooled to 15-30 DEG C, obtains 1,6-naphthalene disulfonate after centrifugal.
2. according to claim 1 a kind of 1,6-naphthalene disulfonate preparation method, is characterized in that: the Tc of solution described in described step 3 is 32-37 DEG C.
3. according to claim 1 a kind of 1,6-naphthalene disulfonate preparation method, is characterized in that: the temperature slowly heating up described in described step 4 is 58-62 DEG C.
4. according to claim 1 a kind of 1,6-naphthalene disulfonate preparation method, is characterized in that: the excellent 18-25 DEG C of the cooling temperature of filtrate described in described step 6.
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| JPS5540648A (en) * | 1978-09-18 | 1980-03-22 | Agency Of Ind Science & Technol | Selective production of 1,6-naphthalenedisolfonic acid |
| JPS6360962A (en) * | 1986-08-29 | 1988-03-17 | Kawasaki Steel Corp | Production of 2,6-naphthalenedisulfonic acid and 2,7-naphthalenedisulfonic acid |
| CN100540532C (en) * | 2006-10-17 | 2009-09-16 | 江苏华达化工集团有限公司 | A kind of preparation method of 1-naphthalenesulfonic acid and 1-naphthalenesulfonic acid sodium salt |
| CN101412686A (en) * | 2008-11-12 | 2009-04-22 | 扬州大学 | Method for preparing 2,7-naphthalenedisulfonate with reaction mother liquor for producing 1,6-naphthalene disulfonic acid |
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