CN103360285A - Production technology of dispersing agent MF (melamine-formaldehyde resin) - Google Patents
Production technology of dispersing agent MF (melamine-formaldehyde resin) Download PDFInfo
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- CN103360285A CN103360285A CN2013102859871A CN201310285987A CN103360285A CN 103360285 A CN103360285 A CN 103360285A CN 2013102859871 A CN2013102859871 A CN 2013102859871A CN 201310285987 A CN201310285987 A CN 201310285987A CN 103360285 A CN103360285 A CN 103360285A
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Abstract
The invention discloses a production technology of dispersing agent MF (melamine-formaldehyde resin). The production technology is carried out by the following steps: leading sulfur trioxide to naphthalene materials to carry out sulfonation reaction; adding formaldehyde water solution to carry out condensation reaction; adding liquid caustic soda to adjust pH to a neutral state; filtering to obtain dispersing agent MF water solution; drying to obtain solid powder dispersing agent MF. The production technology is simple in procedure, and convenient to operate; compared with the traditional technology, sulfuric acid does not need to be added to a naphthalene compound while sulfur trioxide is directly led to carry out sulfonation. Thus, the material cost is saved; meanwhile, the process is simplified; environmental pollution and a potential safety hazard caused by treatment of concentrated sulfuric acid are avoided; no solid waste residue is generated.
Description
Technical field
The present invention relates to dye dispersant MF(condensation compound of methyl naphthalene sulfonic acid and formaldehyde or naphthalene sulfonic acidformaldehyde condensation product) production technique.
Background technology
Dispersant MF mainly is used as dispersion agent and the weighting agent of vat dyes and dispersed dye, be mainly used in dispersed dye, machining agent and dispersion agent when vat dyes grinds, performance is better than dispersion agent N, having mill imitates, dispersiveness, thermotolerance, the stable good advantage of High Temperature Disperse, more high temperature resistant and stable than dispersion agent N.Dispersant MF can make dye shade bright-coloured, look power increases, uniform coloring, can also carry out composite to adapt to the commercialization requirement of various dispersed dye and vat dyes with all kinds of dispersion agents, the early strength water-reducing agent of useful as concrete also, dispersion agent when the dispersion agent in the time of can grinding as vat dyes and the dyeing of vat dyes suspensoid staining, and the auxiliary tanning agent of the stablizer of rubber industry latex, tanning industry.
Mainly be to be that sulphonating agent is produced MF with the vitriol oil (98%) and oleum in the market, sulfonation reaction itself is reversible reaction, make sulfonation complete, must use excessive acid-respons, having a large amount of free acids in the material exists, in order to control the sodium sulphate content in the product, must neutralize this part unnecessary sulfuric acid with lime, will produce a large amount of solid slags like this, process cumbersome, making sulphonating agent with sulphur trioxide is good replacement scheme, can simplify reaction process, does not produce solid slag.China Patent No. is: CN102746196A discloses a kind of technique of making sulphonating agent production Dispersant MF of sulphur trioxide, concrete grammar is to add a certain amount of sulfuric acid first in washing oil (naphthalene or methylnaphthalene), and then pass into sulfur trioxide gas and carry out sulfonation, but need to add the vitriol oil in this technical scheme, technique is complicated, and raw materials cost is higher.
Summary of the invention
Technical problem to be solved by this invention provides the production technique of simple, the easy to operate Dispersant MF of a kind of operation.
In order to realize purpose of the present invention, technical scheme provided by the invention: a kind of production technique of Dispersant MF, carry out according to the following steps:
1. sulphur trioxide being passed into naphthalene is to carry out sulfonation reaction in the raw material;
2. add formalin and carry out condensation reaction;
3. add liquid caustic soda and regulate PH to neutral;
4. get the Dispersant MF aqueous solution after filtering;
5. obtain the pressed powder Dispersant MF after the oven dry.
Preferably, described step 1. in the volumetric concentration of sulphur trioxide be 4%-10%.
Preferably, described sulfonation reaction is carried out in sulfonation reactor.
Preferably, described sulfonation reactor is connected with the graphite condensing works.
Preferably, described naphthalene is that raw material is washing oil or methylnaphthalene.
Dispersant MF is the formaldehyde condensation products of methyl naphthalene sulfonic acid sodium, and chemical constitution is dispersing agent MF, and molecular formula is C23H18O6S2Na2 or (C10H8O3SCH2O) xxNa.
Adopt the beneficial effect of above technical scheme to be: operation of the present invention is simple, easy to operate, compare traditional technology, need not in naphthalene series compound, to add sulfuric acid, carry out sulfonation but directly pass into sulphur trioxide, both saved raw materials cost, simplified simultaneously technique, avoided processing environmental pollution and the potential safety hazard of bringing because of the vitriol oil, and produced without solid slag.
It is too violent that the sulphur trioxide that 4%-10% gas is dense can avoid high dense sulphur trioxide to pass into afterreaction, can allow sufficient reacting carry out simultaneously, guarantees the homogeneity of reaction.But sulfonation reactor sulfonic acid can be in reactor circulating reaction repeatedly, can control simultaneously the physical and chemical parameter of sulfonation reaction, improve reaction efficiency, allow reaction carry out to greatest extent, the cold doubtful device of graphite mainly is the material of carrying secretly in the cold doubtful tail gas, avoid entering atmosphere pollution in the air, and improve the utilization ratio of raw material.
Description of drawings
The schema of Fig. 1 technique of the present invention;
Fig. 2 is the structural representation of sulfonation reactor among the present invention;
Fig. 3 is the vertical view of sulfonation reactor among the present invention;
Among the figure: the 1--reactor, the 2--feed-pipe, the 3--discharge port, the 4--blow-down pipe, 5--and stream pipe, the 6--ventpipe, the 7--opening for feed, the 8--circulating line, the 9--baiting valve, the 10--vomit pipe, the 11--baiting valve, 12--reaction clamp cover, the 13--steam entry, the 14--steam outlet, the 15--cooling water inlet, the 16--cooling water outlet, 17--also flows jacket pipe, the 18--cooling water inlet, the 19--cooling water outlet, the 20--recycle pump, 21--also flows valve, the 22--thief hole, the 23--stopple coupon, the 24-sampling valve, the 25--shower nozzle, the 26--porthole, the 27--agitator, the 28--thermowell.
Embodiment
The principal reaction principle of Dispersant MF production technique:
1) sulfonation
2) condensation
3) neutralization:
Sulfonation reactor among the present invention, Figure 2 shows that the structural representation of sulfonation reactor, the reactor 1 that comprises sealing, reactor 1 top is provided with a plurality of feed-pipes 2, reactor 1 bottom is provided with discharge port 3, the top of reactor 1 vertically is provided with blow-down pipe 4, reactor 1 top also vertically is provided with and flows and manage 5, and stream is managed 5 top seals and is provided with ventpipe 6, and stream pipe 5 sidewalls are provided with opening for feed 7, be connected with circulating line 8 between opening for feed 7 and the discharge port 3, end near discharge port 7 on the circulating line 8 is provided with baiting valve 9, also be provided with vomit pipe 10 on the circulating line 8, vomit pipe 10 is provided with baiting valve 11, reactor 1 is provided with the temperature of reaction control device, and stream pipe 5 is provided with and flow cooling device, the temperature of reaction control device comprises the reaction jacket pipe 12 that is socketed on reactor 1 outer side wall, the outer side wall top of reaction jacket pipe 12 is provided with steam entry 13 and cooling water outlet 16, the outer side wall below of reaction jacket pipe 12 is provided with steam outlet 14 and cooling water inlet 15, be provided with the cooling water circulation pipeline that connects cooling water inlet 15 and cooling water outlet 16 in the reaction jacket pipe 12, also be provided with the water steam pipeline that connects steam entry 13 and steam outlet 14 in the reaction jacket pipe 12, and flow cooling device comprise be socketed on and flow pipe 5 outer side walls and flow jacket pipe 17, and the outer side wall top of stream jacket pipe 17 is provided with cooling water outlet 19, and the outer side wall below of stream jacket pipe 17 is provided with cooling water inlet 18, circulating line 8 is provided with recycle pump 20, recycle pump 20 is arranged on the circulating line 8 between discharge port 3 and the vomit pipe 10, also be provided with on the circulating line 8 and flow valve 21, and stream valve 21 is arranged on the circulating line 8 away from vomit pipe 10 1 sides, circulating line 8 is provided with thief hole 22, thief hole 22 is connected with stopple coupon 23, stopple coupon 23 is provided with sampling valve 24, circulating line 8 is provided with shower nozzle 25 near an end of opening for feed 7, shower nozzle 25 is positioned at and flows pipe 5, shower nozzle 25 arranges vertically downward, and stream pipe 5 sidewalls are provided with porthole 26, porthole 26 is coated with glass, Fig. 3 is the vertical view of sulfonation reactor, reactor 1 is provided with agitator 27 at axis direction, and reactor 2 is provided with the thermowell 28 that vertically passes the top.
Further specify by the following examples the present invention.These embodiment only are the purpose of explanation, and the present invention does not limit these embodiment.
Embodiment 1:
1) sulfonation: the 70g industrial washing oil is put in the sulfonation reactor, then slowly passing into volumetric concentration is 4% sulfur trioxide gas 35g, controlling temperature of reaction by above-mentioned sulfonation reactor is 110-115 ℃, the time of passing into is about 2 hours, after ventilation finishes, is warming up to 130 ℃ after being incubated 1 hour again, under this temperature, continue reaction 3-4 hour, resampling detects solution acidity, is cooled to 110 ℃ after acidity is qualified, passes into the hydrolytic condensation tank;
2) condensation: after temperature was down to 75 ℃, adding 35g concentration was formalin, is warming up to 115 ℃, reacts 5-6 hour, passes into the neutralization reaction tank behind the thin up again;
3) neutralization: pass into liquid caustic soda (32% sodium hydroxide solution) and regulate PH to neutral, pass into strainer;
4) filtering drying: namely get the aqueous solution of Dispersant MF behind the filtering and impurity removing, namely get fixedly powder dispersing agent MF after the oven dry, weighing is 135.4g.
Embodiment 2:
1) sulfonation: the 70g industrial washing oil is put in the sulfonation reactor, then slowly passing into volumetric concentration is 7% sulfur trioxide gas 35g, controlling temperature of reaction by above-mentioned sulfonation reactor is 110-115 ℃, the time of passing into is about 2 hours, after ventilation finishes, be warming up to 130 ℃ after being incubated again 1 hour, under this temperature, continue reaction 3-4 hour, resampling detects solution acidity, be cooled to 110 ℃ after acidity is qualified, pass into the hydrolytic condensation tank, the material of carrying secretly in the sulfonation reactor tail gas is condensed into liquid return by the cold doubtful device of graphite and returns sulphonator;
2) condensation: after temperature was down to 75 ℃, adding 35g concentration was formalin, is warming up to 115 ℃, reacts 5-6 hour, passes into the neutralization reaction tank behind the thin up again;
3) neutralization: pass into liquid caustic soda (32% sodium hydroxide solution) and regulate PH to neutral, pass into strainer;
4) filter: namely get the aqueous solution of Dispersant MF behind the filtering and impurity removing, namely get fixedly powder dispersing agent MF after the oven dry, weighing is 137.4g;
In the present embodiment, the sulphur trioxide volumetric concentration that sulfonation reaction passes into is 7%, react evenly in sulfonation reactor, and the Dispersant MF that art breading obtains is compared to embodiment more than 1, and the material of carrying secretly in the condensable recovery tail gas of the cold doubtful device of graphite has the preferably feature of environmental protection and economy.
Embodiment 3:
1) sulfonation: the 70g methylnaphthalene is put in the sulfonation reactor, then slowly passing into volumetric concentration is 9% sulfur trioxide gas 35g, controlling temperature of reaction by above-mentioned sulfonation reactor is 110-115 ℃, the time of passing into is about 2 hours, after ventilation finishes, be warming up to 130 ℃ after being incubated again 1 hour, under this temperature, continue reaction 3-4 hour, resampling detects solution acidity, be cooled to 110 ℃ after acidity is qualified, pass into the hydrolytic condensation tank, the material of carrying secretly in the sulfonation reactor tail gas is condensed into liquid return by the cold doubtful device of graphite and returns sulphonator;
2) condensation: after temperature was down to 75 ℃, adding 35g concentration was formalin, is warming up to 115 ℃, reacts 5-6 hour, passes into the neutralization reaction tank behind the thin up again;
3) neutralization: pass into liquid caustic soda (32% sodium hydroxide solution) and regulate PH to neutral, pass into strainer;
4) filter: namely get the aqueous solution of Dispersant MF behind the filtering and impurity removing, namely get fixedly powder dispersing agent MF after the oven dry, weighing is 141.7g;
In the present embodiment, the naphthalene of employing is that raw material is pure methylnaphthalene, although the Dispersant MF that obtains is more, pure methylnaphthalene raw materials cost is higher, and the dispersion agents that get are not sufficient to offset the cost that has more more, therefore for being lowered into preferably industrial washing oil.
Embodiment 4:
1) sulfonation: the 70g industrial washing oil is put in the sulfonation reactor, then slowly passing into volumetric concentration is 10% sulfur trioxide gas 35g, controlling temperature of reaction by above-mentioned sulfonation reactor is 110-115 ℃, the time of passing into is about 2 hours, after ventilation finishes, be warming up to 130 ℃ after being incubated again 1 hour, under this temperature, continue reaction 3-4 hour, resampling detects solution acidity, be cooled to 110 ℃ after acidity is qualified, pass into the hydrolytic condensation tank, the material of carrying secretly in the sulfonation reactor tail gas is condensed into liquid return by the cold doubtful device of graphite and returns sulphonator;
2) condensation: after temperature was down to 75 ℃, adding 35g concentration was formalin, is warming up to 115 ℃, reacts 5-6 hour, passes into the neutralization reaction tank behind the thin up again;
3) neutralization: pass into liquid caustic soda (32% sodium hydroxide solution) and regulate PH to neutral, pass into strainer;
4) filter: namely get the aqueous solution of Dispersant MF behind the filtering and impurity removing, namely get fixedly powder dispersing agent MF after the oven dry, weighing is 139.5g; In the present embodiment, the sulphur trioxide volumetric concentration that sulfonation reaction passes into is 10%, reacts uniform and stable in sulfonation reactor, and can obtain the Dispersant MF of maximum.
In sum, embodiment 4 is most preferred embodiment.
Above-described only is preferred implementation of the present invention, should be pointed out that for the person of ordinary skill of the art, under the prerequisite that does not break away from the invention design, can also make some distortion and improvement, and these all belong to protection scope of the present invention.
Claims (5)
1. the production technique of a Dispersant MF is characterized in that, carries out according to the following steps:
1. to pass into naphthalene be to carry out sulfonation reaction in the raw material to sulphur trioxide;
2. add formalin and carry out condensation reaction;
3. add liquid caustic soda and regulate PH to neutral;
4. get the Dispersant MF aqueous solution after filtering;
5. obtain the pressed powder Dispersant MF after the oven dry.
2. the production technique of a kind of Dispersant MF according to claim 1 is characterized in that, the described step 1. volumetric concentration of middle sulphur trioxide is 4%-10%.
3. the production technique of a kind of Dispersant MF according to claim 1 is characterized in that, described sulfonation reaction is carried out in sulfonation reactor.
4. the production technique of a kind of Dispersant MF according to claim 3 is characterized in that, described sulfonation reactor is connected with the graphite condensing works.
5. the production technique of a kind of Dispersant MF according to claim 1 is characterized in that, described naphthalene is that raw material is washing oil or methylnaphthalene.
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| CN2013102859871A CN103360285A (en) | 2013-07-09 | 2013-07-09 | Production technology of dispersing agent MF (melamine-formaldehyde resin) |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103613519A (en) * | 2013-12-06 | 2014-03-05 | 安阳市双环助剂有限责任公司 | Production method for dispersing agent XY |
| CN107602429A (en) * | 2017-08-03 | 2018-01-19 | 绍兴齐英膜科技有限公司 | A kind of method that MF production technologies are improved using membrane technology |
| CN109020843A (en) * | 2018-09-20 | 2018-12-18 | 江苏精禾界面科技有限公司 | A kind of naphthalene sulfonate-alkylnaphthalene sulfonate-formaldehyde condensation products preparation method and applications |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS58180466A (en) * | 1982-04-14 | 1983-10-21 | Nippon Soda Co Ltd | Preparation of naphthalenesulfonic acid |
| CN1566083A (en) * | 2003-07-10 | 2005-01-19 | 浙江吉利达化工有限公司 | Method for manufacturing naphthalene sulfonic acid |
| CN101376639A (en) * | 2008-09-28 | 2009-03-04 | 浙江闰土股份有限公司 | Method for coproduction of dispersants MF and sodium sulphite |
| CN102372456A (en) * | 2010-08-26 | 2012-03-14 | 浙江龙盛集团股份有限公司 | Method for preparing naphthalene series additive from low-acidity process waste water |
| CN102746196A (en) * | 2012-07-17 | 2012-10-24 | 浙江闰土股份有限公司 | Sulfonating technique for producing dye dispersant MF (melamine-formaldehyde) |
-
2013
- 2013-07-09 CN CN2013102859871A patent/CN103360285A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS58180466A (en) * | 1982-04-14 | 1983-10-21 | Nippon Soda Co Ltd | Preparation of naphthalenesulfonic acid |
| CN1566083A (en) * | 2003-07-10 | 2005-01-19 | 浙江吉利达化工有限公司 | Method for manufacturing naphthalene sulfonic acid |
| CN101376639A (en) * | 2008-09-28 | 2009-03-04 | 浙江闰土股份有限公司 | Method for coproduction of dispersants MF and sodium sulphite |
| CN102372456A (en) * | 2010-08-26 | 2012-03-14 | 浙江龙盛集团股份有限公司 | Method for preparing naphthalene series additive from low-acidity process waste water |
| CN102746196A (en) * | 2012-07-17 | 2012-10-24 | 浙江闰土股份有限公司 | Sulfonating technique for producing dye dispersant MF (melamine-formaldehyde) |
Non-Patent Citations (1)
| Title |
|---|
| 常松涛: ""高聚合度β-萘磺酸盐甲醛缩合物的合成研究"", 《大庆石油学院工程硕士专业学位论文》, no. 4, 15 April 2010 (2010-04-15) * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103613519A (en) * | 2013-12-06 | 2014-03-05 | 安阳市双环助剂有限责任公司 | Production method for dispersing agent XY |
| CN107602429A (en) * | 2017-08-03 | 2018-01-19 | 绍兴齐英膜科技有限公司 | A kind of method that MF production technologies are improved using membrane technology |
| CN107602429B (en) * | 2017-08-03 | 2020-05-15 | 绍兴齐英膜科技有限公司 | Method for improving MF production process by adopting membrane technology |
| CN109020843A (en) * | 2018-09-20 | 2018-12-18 | 江苏精禾界面科技有限公司 | A kind of naphthalene sulfonate-alkylnaphthalene sulfonate-formaldehyde condensation products preparation method and applications |
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Application publication date: 20131023 |