CN104096509A - Production process of dispersing agent MF - Google Patents

Production process of dispersing agent MF Download PDF

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Publication number
CN104096509A
CN104096509A CN201310113411.7A CN201310113411A CN104096509A CN 104096509 A CN104096509 A CN 104096509A CN 201310113411 A CN201310113411 A CN 201310113411A CN 104096509 A CN104096509 A CN 104096509A
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China
Prior art keywords
reaction
reactor
dispersant
production technology
sulfuric acid
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CN201310113411.7A
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Chinese (zh)
Inventor
张磊
张立功
张向荣
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Quintar Bio Tech Ltd Zhejiang
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Quintar Bio Tech Ltd Zhejiang
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Priority to CN201310113411.7A priority Critical patent/CN104096509A/en
Publication of CN104096509A publication Critical patent/CN104096509A/en
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Abstract

The invention discloses a production process of a dispersing agent MF. The production process includes: placing methylnaphthalene and concentrated sulfuric acid into a reaction kettle, stirring the materials evenly, conducting heating to 125-135DEG C and performing heat preservation for 3-4h; adding water into the reaction kettle to undergo hydrolysis reaction at 90-100DEG C for 25-35min; putting a formaldehyde solution into the reaction kettle to undergo reaction at 95-105DEG C for 0.5-1h; adding CaCl2 into the reaction kettle to undergo reaction at 80-90DEG C for 0.5-1h; putting liquid alkali into the reaction kettle to undergo neutralization to pH of 5-6, and then adding Ca(OH)2 to adjust the pH to 7.5-8.5; conducting filter pressing to remove solid waste residue by a filter pressing device; and drying the reaction product by drying equipment, and performing packaging to obtain a finished product. The dispersing agent MF produced by the invention does not contain quinoline substances, and the production process provided by the invention can effectively shorten the reaction time and improve production efficiency.

Description

The production technology of Dispersant MF
Technical field
The present invention relates to a kind of production technology of Dispersant MF, belong to a kind of auxiliary chemicals.
Background technology
Dispersant MF is the formaldehyde condensation products of methyl naphthalene sulfonic acid sodium, mainly as dispersant and the filler of reducing dye and disperse dyes, and processing agent and dispersant while being mainly used in disperse dyes, reducing dye grinding, performance is better than dispersant N.Dispersant MF has mill imitates, the advantage that dispersiveness, heat resistance, High Temperature Disperse have been stablized.More high temperature resistant and stable than dispersant N.
The common production technology of Dispersant MF be with technical methylnaphthalene (methyl naphthalene content is more than 60%) or washing oil (methyl naphthalene content is more than 25%) through carrying out sulfonation with the concentrated sulfuric acid, again with formalin condensation, then neutralize its remaining sulfuric acid with lime, by NaOH alkaline, then filter out the solid waste such as calcium sulfate, obtain the aqueous solution of condensation compound of methyl naphthalene sulfonic acid and formaldehyde, i.e. Dispersant MF.But this Dispersant MF contains a large amount of quinoline, when this Dispersant MF be applied to dyestuff and application to dying cloth, the cloth of dying with this dyestuff brings very large harm to person health, contacting of this dyestuff and human body, can to human body, cause the possibility of canceration, the countries such as existing West Europe ban use of containing quinoline dispersant at dye industry more.
Publication number is that the Chinese invention patent of 102114396A discloses a kind of production technology without quinoline Dispersant MF, this production technology drops into 16 carbon methyl naphthalenes in reactor, be heated to 50～60 degrees Celsius, again inorganic acid is added, stir one hour, more separated, then 16 refining carbon methyl naphthalenes are heated to 110 degrees Celsius, drip sulfuric acid, be warming up to 130～140 degrees Celsius, carry out sulfonation normal pressure heat-insulating 4 hours.Be cooled to again 110 degrees Celsius, then be hydrolyzed.Be cooled to again under 80 degrees Celsius and drip formaldehyde, be warming up in 105～115 degrees Celsius, normal pressure condensation insulation 3 hours.Add again liquid caustic soda neutralization, then add between lime adjusting pH value to 7～8, then carry out press filtration, then dry packing finished product.The method comparatively bothers inorganic acid separation when actual production, technique more complicated, and the reaction time is long, has improved the production cost of enterprise.
Summary of the invention
The present invention is directed to the deficiencies in the prior art, object is to provide a kind of technique simple, in finished product without the production technology of the Dispersant MF of quinoline.
The technical scheme that the present invention realizes above-mentioned purpose is: a kind of production technology of Dispersant MF, comprises the following steps:
The first step: sulfonating reaction, methyl naphthalene and the concentrated sulfuric acid are put in reactor and stirred, be heated to 125 ~ 135 ℃, be incubated 3 ~ 4 hours;
Second step: hydrolysis, after the first step has been reacted, in reactor, add the water reaction that is hydrolyzed, the temperature of hydrolysis is 90 ~ 100 ℃, reacts 25 ~ 35 minutes;
The 3rd step: condensation reaction after second step has reacted, drops into formalin, 95 ~ 105 ℃ of reaction temperatures, 0.5 ~ 1 hour reaction time in reactor;
The 4th step: go quinoline reaction, after three-step reaction completes, add CaCl in reactor 2, 80 ~ 90 ℃ of reaction temperatures, 0.5 ~ 1 hour reaction time;
The 5th step: neutralization reaction after four-step reaction completes, drops into liquid caustic soda and neutralizes pH5 ~ 6, then adds Ca (OH) in reactor 2be adjusted to pH7.5 ~ 8.5;
The 6th step: press filtration, the material after the 5th step has been reacted is discharged from reactor, with filter-pressing device, solid slag press filtration is removed;
The 7th step: dry, product is dried by drying plant, be packaged into finished product.
Add the percentage by weight of various raw materials in reactor to be, methyl naphthalene: 19.2 ~ 23.4%; The concentrated sulfuric acid: 23.1 ~ 24.3%; Water 12.5 ~ 14.5%; Formaldehyde: 9 ~ 11.6%; CaCl 2: 2 ~ 5.5%; Liquid caustic soda: 17 ~ 18.5%; Ca (OH) 2: 12.2 ~ 14.5%.
The weight percent concentration of the described concentrated sulfuric acid is 98 ~ 98.5%.
The weight percent concentration of described formaldehyde is 34 ~ 35%.
Described liquid caustic soda is NaOH solution, and its weight percent concentration is 28 ~ 29.5%.
Described filter-pressing device comprises squeezer or centrifuge.
Described drying plant comprises vacuum drying oven, double cone dryer or vacuum double cone dryer.
The invention has the beneficial effects as follows: owing to having increased in the present invention the step of going quinoline reaction, by add CaCl in reactant 2make not contain in the Dispersant MF after making quinoline material.Therefore, the Dispersant MF that production technology of the present invention is produced is a kind of chemical products of safety and environmental protection, this product after for dyestuff, the cloth of dying, the clothes of making to human body without any harm; The present invention has also effectively shortened the reaction time, has improved production efficiency, has reduced production cost.
Accompanying drawing explanation
Fig. 1 is production technological process of the present invention.
The specific embodiment
Below in conjunction with accompanying drawing, and in conjunction with the embodiments, the present invention is described further.
Embodiment 1:
A production technology for Dispersant MF, Fig. 1 is production technological process of the present invention.
Production technology comprises the following steps:
The first step: sulfonating reaction, methyl naphthalene and the concentrated sulfuric acid are put in reactor and stirred, be heated to 125 ℃, be incubated 4 hours;
Second step: hydrolysis, after the first step has been reacted, in reactor, add the water reaction that is hydrolyzed, the temperature of hydrolysis is 90 ℃, reacts 35 minutes;
The 3rd step: condensation reaction after second step has reacted, drops into formalin, 95 ℃ of reaction temperatures, 1 hour reaction time in reactor;
The 4th step: go quinoline reaction, after three-step reaction completes, add CaCl in reactor 2, 80 ℃ of reaction temperatures, 1 hour reaction time;
The 5th step: neutralization reaction after four-step reaction completes, drops into liquid caustic soda and neutralizes pH5, then adds Ca (OH) in reactor 2be adjusted to pH7.5;
The 6th step: press filtration, the material after the 5th step has been reacted is discharged from reactor, with filter-pressing device, solid slag press filtration is removed;
The 7th step: dry, product is dried by drying plant, be packaged into finished product.
Add the percentage by weight of various raw materials in reactor to be, methyl naphthalene: 23.4%; The concentrated sulfuric acid: 23.9%; Water: 12.5%; Formaldehyde: 9%; CaCl 2: 2%; Liquid caustic soda: 17%; Ca (OH) 2: 12.2%.
The weight percent concentration of the described concentrated sulfuric acid is 98%.
The weight percent concentration of described formaldehyde is 34%.
Described liquid caustic soda is NaOH solution, and its weight percent concentration is 28%.
Described filter-pressing device comprises squeezer or centrifuge.
Described drying plant comprises vacuum drying oven, double cone dryer or vacuum double cone dryer.
Embodiment 2:
A production technology for Dispersant MF, Fig. 1 is production technological process of the present invention.
Production technology comprises the following steps:
The first step: sulfonating reaction, methyl naphthalene and the concentrated sulfuric acid are put in reactor and stirred, be heated to 135 ℃, be incubated 3 hours;
Second step: hydrolysis, after the first step has been reacted, in reactor, add the water reaction that is hydrolyzed, the temperature of hydrolysis is 100 ℃, reacts 25 minutes;
The 3rd step: condensation reaction after second step has reacted, drops into formalin, 105 ℃ of reaction temperatures, 0.5 hour reaction time in reactor;
The 4th step: go quinoline reaction, after three-step reaction completes, add CaCl in reactor 2, 90 ℃ of reaction temperatures, 0.5 hour reaction time;
The 5th step: neutralization reaction after four-step reaction completes, drops into liquid caustic soda and neutralizes pH6, then adds Ca (OH) in reactor 2be adjusted to pH8.5;
The 6th step: press filtration, the material after the 5th step has been reacted is discharged from reactor, with filter-pressing device, solid slag press filtration is removed;
The 7th step: dry, product is dried by drying plant, be packaged into finished product.
Add the percentage by weight of various raw materials in reactor to be, methyl naphthalene: 19.2%; The concentrated sulfuric acid: 24.3%; Water 14.5%; Formaldehyde: 9.1%; CaCl 2: 2.1%; Liquid caustic soda: 18.5%; Ca (OH) 2: 12.3%.
The weight percent concentration of the described concentrated sulfuric acid is 98.5%.
The weight percent concentration of described formaldehyde is 35%.
Described liquid caustic soda is NaOH solution, and its weight percent concentration is 29.5%.
Described filter-pressing device comprises squeezer or centrifuge.
Described drying plant comprises vacuum drying oven, double cone dryer or vacuum double cone dryer.
Embodiment 3:
A production technology for Dispersant MF, Fig. 1 is production technological process of the present invention.
Production technology comprises the following steps:
The first step: sulfonating reaction, methyl naphthalene and the concentrated sulfuric acid are put in reactor and stirred, be heated to 130 ℃, be incubated 3.5 hours;
Second step: hydrolysis, after the first step has been reacted, in reactor, add the water reaction that is hydrolyzed, the temperature of hydrolysis is 95 ℃, reacts 30 minutes;
The 3rd step: condensation reaction after second step has reacted, drops into formalin, 100 ℃ of reaction temperatures, 0.8 hour reaction time in reactor;
The 4th step: go quinoline reaction, after three-step reaction completes, add CaCl in reactor 2, 85 ℃ of reaction temperatures, 0.8 hour reaction time;
The 5th step: neutralization reaction after four-step reaction completes, drops into liquid caustic soda and neutralizes pH5.5, then adds Ca (OH) in reactor 2be adjusted to pH8;
The 6th step: press filtration, the material after the 5th step has been reacted is discharged from reactor, with filter-pressing device, solid slag press filtration is removed;
The 7th step: dry, product is dried by drying plant, be packaged into finished product.
Add the percentage by weight of various raw materials in reactor to be, methyl naphthalene: 19.2%; The concentrated sulfuric acid: 23.1%; Water: 12.5%; Formaldehyde: 11.6%; CaCl 2: 2.0%; Liquid caustic soda: 17.1%; Ca (OH) 2: 14.5%.
The weight percent concentration of the described concentrated sulfuric acid is 98.5%.
The weight percent concentration of described formaldehyde is 35%.
Described liquid caustic soda is NaOH solution, and its weight percent concentration is 29.5%.
Described filter-pressing device comprises squeezer or centrifuge.
Described drying plant comprises vacuum drying oven, double cone dryer or vacuum double cone dryer.
Embodiment 4:
A production technology for Dispersant MF, Fig. 1 is production technological process of the present invention.
Production technology comprises the following steps:
The first step: sulfonating reaction, methyl naphthalene and the concentrated sulfuric acid are put in reactor and stirred, be heated to 132 ℃, be incubated 3.6 hours;
Second step: hydrolysis, after the first step has been reacted, in reactor, add the water reaction that is hydrolyzed, the temperature of hydrolysis is 96 ℃, reacts 30 minutes;
The 3rd step: condensation reaction after second step has reacted, drops into formalin, 102 ℃ of reaction temperatures, 0.75 hour reaction time in reactor;
The 4th step: go quinoline reaction, after three-step reaction completes, add CaCl in reactor 2, 87 ℃ of reaction temperatures, 0.75 hour reaction time;
The 5th step: neutralization reaction after four-step reaction completes, drops into liquid caustic soda and neutralizes pH5.7, then adds Ca (OH) in reactor 2be adjusted to pH8.2;
The 6th step: press filtration, the material after the 5th step has been reacted is discharged from reactor, with filter-pressing device, solid slag press filtration is removed;
The 7th step: dry, product is dried by drying plant, be packaged into finished product.
Add the percentage by weight of various raw materials in reactor to be, methyl naphthalene: 19.4%; The concentrated sulfuric acid: 23.3%; Water: 12.6%; Formaldehyde: 9.2%; CaCl 2: 5.5%; Liquid caustic soda: 17.5%; Ca (OH) 2: 12.5%.
The weight percent concentration of the described concentrated sulfuric acid is 98.5%.
The weight percent concentration of described formaldehyde is 35%.
Described liquid caustic soda is NaOH solution, and its weight percent concentration is 29.5%.
Described filter-pressing device comprises squeezer or centrifuge.
Described drying plant comprises vacuum drying oven, double cone dryer or vacuum double cone dryer.
Embodiment 5:
A production technology for Dispersant MF, Fig. 1 is production technological process of the present invention.
Production technology comprises the following steps:
The first step: sulfonating reaction, methyl naphthalene and the concentrated sulfuric acid are put in reactor and stirred, be heated to 132 ℃, be incubated 3.6 hours;
Second step: hydrolysis, after the first step has been reacted, in reactor, add the water reaction that is hydrolyzed, the temperature of hydrolysis is 96 ℃, reacts 30 minutes;
The 3rd step: condensation reaction after second step has reacted, drops into formalin, 102 ℃ of reaction temperatures, 0.75 hour reaction time in reactor;
The 4th step: go quinoline reaction, after three-step reaction completes, add CaCl in reactor 2, 87 ℃ of reaction temperatures, 0.75 hour reaction time;
The 5th step: neutralization reaction after four-step reaction completes, drops into liquid caustic soda and neutralizes pH5.7, then adds Ca (OH) in reactor 2be adjusted to pH8.2;
The 6th step: press filtration, the material after the 5th step has been reacted is discharged from reactor, with filter-pressing device, solid slag press filtration is removed;
The 7th step: dry, product is dried by drying plant, be packaged into finished product.
Add the percentage by weight of various raw materials in reactor to be, methyl naphthalene: 20.4%; The concentrated sulfuric acid: 23.3%; Water: 12.6%; Formaldehyde: 10.2%; CaCl 2: 3.5%; Liquid caustic soda: 17.5%; Ca (OH) 2: 12.5%.
The weight percent concentration of the described concentrated sulfuric acid is 98.5%.
The weight percent concentration of described formaldehyde is 35%.
Described liquid caustic soda is NaOH solution, and its weight percent concentration is 29%.
Described filter-pressing device comprises squeezer or centrifuge.
Described drying plant comprises vacuum drying oven, double cone dryer or vacuum double cone dryer.

Claims (7)

1. the production technology of Dispersant MF, is characterized in that comprising the following steps:
The first step: sulfonating reaction, methyl naphthalene and the concentrated sulfuric acid are put in reactor and stirred, be heated to 125 ~ 135 ℃, be incubated 3 ~ 4 hours;
Second step: hydrolysis, after the first step has been reacted, in reactor, add the water reaction that is hydrolyzed, the temperature of hydrolysis is 90 ~ 100 ℃, reacts 25 ~ 35 minutes;
The 3rd step: condensation reaction after second step has reacted, drops into formalin, 95 ~ 105 ℃ of reaction temperatures, 0.5 ~ 1 hour reaction time in reactor;
The 4th step: go quinoline reaction, after three-step reaction completes, add CaCl in reactor 2, 80 ~ 90 ℃ of reaction temperatures, 0.5 ~ 1 hour reaction time;
The 5th step: neutralization reaction after four-step reaction completes, drops into liquid caustic soda and neutralizes pH5 ~ 6, then adds Ca (OH) in reactor 2be adjusted to pH7.5 ~ 8.5;
The 6th step: press filtration, the material after the 5th step has been reacted is discharged from reactor, with filter-pressing device, solid slag press filtration is removed;
The 7th step: dry, product is dried by drying plant, be packaged into finished product.
2. the production technology of Dispersant MF as claimed in claim 1, is characterized in that: add the percentage by weight of various raw materials in reactor to be, methyl naphthalene: 19.2 ~ 23.4%; The concentrated sulfuric acid: 23.1 ~ 24.3%; Water: 12.5 ~ 14.5%; Formaldehyde: 9 ~ 11.6%; CaCl 2: 2 ~ 5.5%; Liquid caustic soda: 17 ~ 18.5%; Ca (OH) 2: 12.2 ~ 14.5%.
3. the production technology of Dispersant MF as claimed in claim 1, is characterized in that: the weight percent concentration of the described concentrated sulfuric acid is 98 ~ 98.5%.
4. the production technology of Dispersant MF as claimed in claim 1, is characterized in that: the weight percent concentration of described formaldehyde is 34 ~ 35%.
5. the production technology of Dispersant MF as claimed in claim 1, is characterized in that: described liquid caustic soda is NaOH solution, and its weight percent concentration is 28 ~ 29.5%.
6. the production technology of Dispersant MF as claimed in claim 1, is characterized in that: described filter-pressing device comprises squeezer or centrifuge.
7. the production technology of Dispersant MF as claimed in claim 1, is characterized in that: described drying plant comprises vacuum drying oven, double cone dryer or vacuum double cone dryer.
CN201310113411.7A 2013-04-02 2013-04-02 Production process of dispersing agent MF Pending CN104096509A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105541672A (en) * 2015-12-15 2016-05-04 浙江闰土研究院有限公司 Clean production process of dye dispersant MF
CN105712906A (en) * 2016-03-29 2016-06-29 绍兴文理学院 Method for preparing high-quality dispersing agent MF with reactive distillation method
CN106336338A (en) * 2015-07-09 2017-01-18 上海宝钢化工有限公司 Method for removing quinoline in DMNO-3
CN112375019A (en) * 2020-11-25 2021-02-19 济宁碳素集团有限公司 Method for producing environment-friendly low-quinoline MF dispersant by using ethylene tar

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Publication number Priority date Publication date Assignee Title
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CN102114396A (en) * 2010-12-10 2011-07-06 江阴市盛通化工有限公司 Non-quinoline dispersant MF and production process
CN102662010A (en) * 2012-05-03 2012-09-12 安阳市双环助剂有限责任公司 Method for measuring quinoline content in dispersing agent MF

Patent Citations (3)

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Publication number Priority date Publication date Assignee Title
US4324704A (en) * 1978-12-15 1982-04-13 International Flavors & Fragrances Inc. Process for hydrogenation of damascenone, products produced thereby and organoleptic uses of said products
CN102114396A (en) * 2010-12-10 2011-07-06 江阴市盛通化工有限公司 Non-quinoline dispersant MF and production process
CN102662010A (en) * 2012-05-03 2012-09-12 安阳市双环助剂有限责任公司 Method for measuring quinoline content in dispersing agent MF

Non-Patent Citations (2)

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曹泽环等: "扩散剂 MF 工艺技术改革的探索", 《青岛科技大学学报(自然科学版)》, no. 01, 30 June 1985 (1985-06-30), pages 16 - 23 *

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106336338A (en) * 2015-07-09 2017-01-18 上海宝钢化工有限公司 Method for removing quinoline in DMNO-3
CN105541672A (en) * 2015-12-15 2016-05-04 浙江闰土研究院有限公司 Clean production process of dye dispersant MF
CN105541672B (en) * 2015-12-15 2017-06-20 浙江闰土研究院有限公司 A kind of process for cleanly preparing of dye dispersant MF
CN105712906A (en) * 2016-03-29 2016-06-29 绍兴文理学院 Method for preparing high-quality dispersing agent MF with reactive distillation method
CN105712906B (en) * 2016-03-29 2017-10-10 绍兴文理学院 A kind of method that reaction rectification method prepares high-quality Dispersant MF
CN112375019A (en) * 2020-11-25 2021-02-19 济宁碳素集团有限公司 Method for producing environment-friendly low-quinoline MF dispersant by using ethylene tar

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Application publication date: 20141015