CN110256303A - Dispersant MF and preparation method thereof - Google Patents
Dispersant MF and preparation method thereof Download PDFInfo
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- CN110256303A CN110256303A CN201910605949.7A CN201910605949A CN110256303A CN 110256303 A CN110256303 A CN 110256303A CN 201910605949 A CN201910605949 A CN 201910605949A CN 110256303 A CN110256303 A CN 110256303A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C303/00—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides
- C07C303/02—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of sulfonic acids or halides thereof
- C07C303/04—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of sulfonic acids or halides thereof by substitution of hydrogen atoms by sulfo or halosulfonyl groups
- C07C303/06—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of sulfonic acids or halides thereof by substitution of hydrogen atoms by sulfo or halosulfonyl groups by reaction with sulfuric acid or sulfur trioxide
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C303/00—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides
- C07C303/02—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of sulfonic acids or halides thereof
- C07C303/22—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of sulfonic acids or halides thereof from sulfonic acids, by reactions not involving the formation of sulfo or halosulfonyl groups; from sulfonic halides by reactions not involving the formation of halosulfonyl groups
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C303/00—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides
- C07C303/32—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of salts of sulfonic acids
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K23/00—Use of substances as emulsifying, wetting, dispersing, or foam-producing agents
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Abstract
The present invention provides a kind of Dispersant MF and preparation method thereof.The preparation method comprises the following steps: mixing step: naphthalene series compound being added dropwise in sulfuric acid system, mix products are obtained；Sulfonation procedure: the mix products are subjected to insulation reaction, obtain sulfonated products；Hydrolysing step: being added water in the sulfonated products, and reaction is hydrolyzed, obtains hydrolysate；Condensation step: being added formaldehyde in the hydrolysate, carries out condensation reaction, obtains condensation product.Of the invention preparation method is simple, and is suitable for producing in enormous quantities, and the whiteness of Dispersant MF that the present invention is prepared is high, and contamination is excellent, suitable for preparing dyestuff.
Description
Technical field
The present invention relates to a kind of Dispersant MFs and preparation method thereof, belong to weaving chemical field.
Background technique
Dispersant MF (formaldehyde condensation products of naphthalene series compound sulfonic acid) is a kind of anionic surfactant, is mainly used as point
Dissipate the dispersing agent and filler of dyestuff and reducing dye.There is mill to imitate for it, and dispersibility, heat resistance, High Temperature Dispersion Stability are good
The advantages of, it can be compounded with all kinds of dispersing agents to adapt to the commercial requirements of various disperse dyes and reducing dye.
It is essentially all with naphthalene system chemical combination though domestic Dispersant MF production technology is various at present, similar
Object is substrate, and at a certain temperature, the sulfuric acid that various concentration is added dropwise carries out sulfonating reaction, and sulfonating reaction terminates, hydrolyzed, contracted
Close, neutralize etc. processes and be made.The Dispersant MF being prepared using this method, contamination are serious.
Citation [1] provides a kind of production technology of Dispersant MF.Naphthalene series compound and the concentrated sulfuric acid are put into instead
It answers in kettle and stirs evenly, be heated to 125~135 DEG C, keep the temperature 3~4 hours；Water is added in a kettle, reaction, water is hydrolyzed
The temperature of solution reaction is 90~100 DEG C, is reacted 25~35 minutes；Formalin, reaction temperature 90~105 are put into a kettle
DEG C, the reaction time 0.5~1 hour；CaCl is added in a kettle2, 80~90 DEG C of reaction temperature, the reaction time 0.5~1 is small
When；Investment liquid alkaline is neutralized to pH5~6 in a kettle, adds Ca (OH)2It is adjusted to pH7.5~8.5；It will from filter-pressing device
Solid slag filters pressing removes；Reaction product is dried by drying equipment, is packaged into finished product.This method is because be by naphthalene system chemical combination
Object and the concentrated sulfuric acid are put into reaction kettle simultaneously to stir evenly, and the contamination for the Dispersant MF being prepared is poor.
Citation [2] provides a kind of quinoline-free dispersing agent MF and production technology, main component packet in the Dispersant MF
It includes weight percent and is respectively as follows: 35% α-naphthalene series compound sulfonic formaldehyde condensation compound and 65% β-naphthalene series compound sulfonic acid
Formaldehyde condensation products.Its production technology are as follows: 16 carbon methyl naphthalenes are put into reaction kettle, are heated to 50~60 degrees Celsius, then by nothing
Machine acid is added, and stirs one hour, then separates and then 16 carbon naphthalene series compounds of purification are heated to 110 degrees Celsius, and sulphur is added dropwise
Acid is warming up to 130~140 degrees Celsius, carries out sulfonation normal pressure heat-insulating 4 hours.110 degrees Celsius are cooled to, then is hydrolyzed.Again
It is cooled under 80 degrees Celsius and formaldehyde is added dropwise, is warming up in 105~115 degrees Celsius, normal pressure condensation heat preservation 3 hours.Liquid feeding alkali is carried out again
Neutralize, then plus lime adjust pH value between 7~8, then carry out filters pressing, then dry packing finished product.This method is by the concentrated sulfuric acid
It is added dropwise in 16 carbon naphthalene series compounds, the contamination for the Dispersant MF being prepared is poor.
Citation [1]: CN104096509A
Citation [2]: CN102114396A
Summary of the invention
Problems to be solved by the invention
In view of the technical problems existing in the prior art, present invention firstly provides a kind of preparation methods of Dispersant MF.
Of the invention preparation method is simple, and is suitable for producing in enormous quantities, and the contamination of Dispersant MF that the present invention is prepared
Property is excellent, suitable for preparing dyestuff.
Further, the present invention also provides a kind of Dispersant MFs, and the whiteness of the Dispersant MF is high, and contamination is excellent.
The solution to the problem
Present invention firstly provides a kind of preparation methods of Dispersant MF comprising following steps:
Mixing step: naphthalene series compound is added dropwise in sulfuric acid system, obtains mix products；
Sulfonation procedure: the mix products are subjected to insulation reaction, obtain sulfonated products；
Hydrolysing step: being added water in the sulfonated products, and reaction is hydrolyzed, obtains hydrolysate；
Condensation step: being added formaldehyde in the hydrolysate, carries out condensation reaction, obtains condensation product.
Preparation method according to the present invention, wherein the temperature of the mixing step be 40 DEG C or more, preferably 40~125
℃；And/or
The concentration of the sulfuric acid is 98% or more, and preferred concentration is 98%~104.5%.
Preparation method according to the present invention, wherein in the mixing step, the molar ratio of the naphthalene series compound and sulfuric acid
For 1:1.1~1.6, preferably 1:1.3~1.6.
Preparation method according to the present invention, wherein in the sulfonation procedure, the insulation reaction is in the presence of steam
It carries out；
And/or the temperature of the insulation reaction is 130~180 DEG C, the time of the insulation reaction is 3~5h.
Preparation method according to the present invention, wherein in sulfonation procedure, when carrying out insulation reaction, while utilizing vacuum
Dewatering process is to remove the water generated during insulation reaction；Preferably, in the vacuum dewatering technique, vacuum degree is
0.04MPa or more.
Preparation method according to the present invention, wherein in the hydrolysing step, the temperature of hydrolysis is 115~130 DEG C,
Preferably 120~128 DEG C；And/or
After the hydrolysis, the acid value of hydrolysate is 20~25%, preferably 22~23%.
Preparation method according to the present invention, wherein in the condensation step, temperature when formaldehyde is added in hydrolysate
It is 75~80 DEG C；The temperature of condensation reaction is 100~120 DEG C；And/or
The molar ratio of formaldehyde and naphthalene series compound is 0.7~0.8:1.
The present invention also provides a kind of Dispersant MFs, wherein the preparation method of the Dispersant MF through the invention is prepared into
It arrives；The whiteness of the Dispersant MF is 25 or more, preferably 25-40.
Dispersant MF according to the present invention, wherein the whiteness detects obtain by the following method:
The cloth after drawing a design is taken, the whiteness value of the cloth specimen is measured using spectrophotometric color measurement instrument.
The effect of invention
Of the invention preparation method is simple, and is suitable for producing in enormous quantities, and the dispersing agent that the present invention is prepared
The whiteness of MF is high, and contamination is excellent, suitable for preparing dyestuff.
Further, the whiteness of Dispersant MF of the invention is high, and contamination is excellent.
Specific embodiment
It will be detailed below various exemplary embodiments, feature and aspect of the invention.Dedicated word " example herein
Property " mean " being used as example, embodiment or illustrative ".Here as any embodiment illustrated by " exemplary " should not necessarily be construed as
Preferred or advantageous over other embodiments.
In addition, in order to better illustrate the present invention, numerous details is given in specific embodiment below.
It will be appreciated by those skilled in the art that without certain details, the present invention equally be can be implemented.In other example,
Method well known to those skilled in the art, means, equipment and step are not described in detail, in order to highlight master of the invention
Purport.
Such as without Special Statement, unit used in the present invention is SI units, and the number occurred in the present invention
Value, numberical range should all be interpreted as containing the inevitable Systematic Errors of institute in industrial production.
First embodiment
First embodiment of the invention provides a kind of preparation method of Dispersant MF, comprising the following steps:
Mixing step: naphthalene series compound is added dropwise in sulfuric acid system, obtains mix products；
Sulfonation procedure: the mix products are subjected to insulation reaction, obtain sulfonated products；
Hydrolysing step: being added water in the sulfonated products, and reaction is hydrolyzed, obtains hydrolysate；
Condensation step: being added formaldehyde in the hydrolysate, carries out condensation reaction, obtains condensation product.
Preparation method is simple for Dispersant MF of the invention, and is suitable for producing in enormous quantities, and the present invention is prepared into
The whiteness of the Dispersant MF arrived is high, and contamination is excellent, suitable for preparing dyestuff.Specifically:
Mixing step
It is that naphthalene series compound is added dropwise in sulfuric acid system in mixing step of the invention.By the way that naphthalene series compound is dripped
It adds in sulfuric acid system, so as to effectively improve the whiteness and contamination of Dispersant MF.
In the present invention, naphthalene series compound is usually methyl naphthalene, such as: it can be technical methylnaphthalene, industrial washing oil, industry
The combination of one or more of naphthalene, alpha-methyl-naphthalene, beta-methylnaphthalene etc..
Specifically, in the present invention, in order to reduce production cost, technical methylnaphthalene can be used and/or industrial washing oil is made
For naphthalene series compound.Wherein, technical methylnaphthalene is usually the colourless oily liquids to yellowish-brown, mainly alpha-methyl-naphthalene and β-first
The mixture of base naphthalene.Industrial washing oil is usually the absorption oil that benzene or naphthalene series compound are washed out from coal gas, generally yellowish-brown or
Brown oil liquid.Industrial washing oil is mainly made of naphthalene compounds, acenaphthene, fluorenes, dibenzofuran, phenol, nitrogen heteroaromatic rings compound etc..
In order to make to react better progress, the concentration of sulfuric acid of the invention is 98% or more, preferred concentration is 98%~
104.5%.That is, sulfuric acid of the invention can be the concentrated sulfuric acid and/or oleum.In the concentrated sulfuric acid, the quality point of sulfuric acid
Number is generally between 98~100%.Oleum, that is, the sulfuric acid solution of sulfur trioxide.In oleum, the matter of sulfuric acid
Score is measured generally between 100~104.5%.
In the mixing step, the molar ratio of the naphthalene series compound and sulfuric acid is 1:1.1~1.6, preferably 1:1.3~
1.6, such as: the molar ratio of the naphthalene series compound and sulfuric acid is 1:1.2,1:1.4,1:1.5 etc..When the naphthalene series compound with
When the molar ratio of sulfuric acid is 1:1.1~1.6, be conducive to the progress of later period sulfonating reaction.In addition, the temperature of the mixing step is
40 DEG C or more, preferably 40~125 DEG C, such as: the temperature of mixing step can be 50 DEG C, and 60 DEG C, 70 DEG C, 80 DEG C, 90 DEG C,
100 DEG C, 110 DEG C etc., naphthalene series compound can be made tentatively to be mixed with sulfuric acid, be conducive to the progress of later period sulfonating reaction.
Sulfonation procedure
The sulfonating reaction of the invention is that the mix products are carried out insulation reaction, obtain sulfonated products.
In the present invention, insulation reaction is carried out in the presence of steam, sulfonating reaction can be made relatively stable into
Row, and reaction temperature can be more effectively controlled, so as to make the more sufficient fully reacting of sulfuric acid, after completion of the reaction,
A small amount of sulfuric acid is only deposited in solution.
Further, in sulfonation procedure, when carrying out insulation reaction, while using vacuum dewatering technique to remove insulation reaction
The water generated in the process；Preferably, in the vacuum dewatering technique, vacuum degree is 0.04MPa or more.In general, described true
Reciprocal of duty cycle can be 0.05MPa, 0.06MPa, 0.07MPa, 0.08MPa, 0.09MPa, 0.1MPa etc..
The temperature and time of the insulation reaction, which can according to need, to be set, preferably, the temperature of insulation reaction
It can be 130~180 DEG C, such as the temperature of insulation reaction can be 135 DEG C, 140 DEG C, 145 DEG C, 150 DEG C, 155 DEG C etc.；Heat preservation
The time of reaction can be 3~5h, such as can be 3.5h, 4h, 4.5h etc..
Hydrolysing step
In the present invention, it after sulfonated reaction, needs that water is added in the sulfonated products, reaction is hydrolyzed, obtains
Hydrolysate.
After the hydrolysis, the acid value of hydrolysate is 20~25%, preferably 22~23%.Such as the acid of hydrolysate
Value can be 21%, 21.5%, 22.5%, 23.5%, 24% etc., and in the present invention, acid value can be expressed as institute in hydrolysate
The mass fraction of the sulfuric acid shown.
In hydrolysing step, the temperature of hydrolysis can be 115~130 DEG C, preferably 120~128 DEG C.To advantageous
In the progress of condensation step.
Condensation step
In the present invention, hydrolysate and formaldehyde can be subjected to condensation reaction and obtains condensation product.Wherein, the condensation
In step, temperature when formaldehyde being added in hydrolysate is 75~80 DEG C；The temperature of condensation reaction is 100~120 DEG C.At this
In invention, the molar ratio of formaldehyde and naphthalene series compound is 0.7~0.8:1.When the molar ratio of formaldehyde and naphthalene series compound be 0.7~
When 0.8:1, condensation reaction can be made complete.
Neutralization procedure
After the condensation step, the present invention further preferably includes neutralization procedure.Neutralization procedure is using the base extraction condensation
Product, to carry out neutralization reaction.PH value after neutralization reaction is 6~9, such as pH value can be 6.5,7,7.5,8 etc., thus
To corresponding Dispersant MF.
In the present invention, calcium carbonate and lime etc. can not be added in lye influences the alkaline agent of dye dispersant quality, i.e.,
Neutralization reaction can be achieved, be further reduced the content of waste residue.In the present invention, lye can be NaOH aqueous solution (liquid alkaline) etc.,
The pH value of the neutralized reaction product obtained after neutralization is between 6~9, such as pH value can be 6.5,7,7.5,8 etc..
In addition, can use urea in order to improve the purity of Dispersant MF and remove excessive formaldehyde, enable to the present invention
Dispersant MF safety it is higher.
Second embodiment
The present invention also provides a kind of Dispersant MFs, wherein the preparation method of the Dispersant MF through the invention is prepared into
It arrives；The whiteness of the Dispersant MF is 25 or more, preferably 25-40.Whiteness numerical value is bigger, contamination of the Dispersant MF to cloth
It is smaller, Dispersant MF contamination is evaluated using whiteness index, avoids artificial subjective factor, it is more accurate to grade.
Specifically, Dispersant MF of the invention, drawn a design using terylene cloth test when, the whiteness of the Dispersant MF is
25 or more, preferably 25-40；Drawn a design using cotton cloth test when, the whiteness of the Dispersant MF is 25 or more, preferably 27
More than, more preferably 27-40.
Further, whiteness of the present invention detects obtain by the following method:
The cloth after drawing a design is taken, the whiteness of the cloth specimen is measured using spectrophotometric color measurement instrument.
Embodiment
Embodiment of the present invention is described in detail below in conjunction with embodiment, but those skilled in the art will
Understand, the following example is merely to illustrate the present invention, and should not be taken as limiting the scope of the invention.It is not specified in embodiment specific
Condition person carries out according to conventional conditions or manufacturer's recommended conditions.Reagents or instruments used without specified manufacturer is
It can be with conventional products that are commercially available.
Embodiment 1
A. the oleum 2400kg that 104.5% is put into the reaction kettle of 5000L, then heats to 45 DEG C, starts to delay
Slow that technical methylnaphthalene 2400kg is added dropwise, with the dropwise addition of technical methylnaphthalene, system temperature is gradually risen, and control dropping temperature is lower than
125 DEG C, drop finishes within about 4 hours, technical methylnaphthalene completion of dropwise addition, opens steam and is slowly warming up to 150 DEG C or so, while opening true
Sky maintains vacuum degree in 0.05MPa or so, insulation reaction 3h；
B. sulfonation terminates, and is cooled to 125 DEG C, 800kg water is slowly added dropwise, reaction is hydrolyzed, and hydrolysis terminates, and surveys acid value
22.83%；
C. hydrolysis terminates, and is discharged to condensation kettle, continues to be cooled to 75~80 DEG C, and the first that mass fraction is 37% is then added
Aldehyde 1000kg is finished and is to slowly warm up to 105 DEG C of progress condensation reaction 3h；
D. after condensation reaction, being neutralized to pH with liquid alkaline is 6.5, adds urea 200kg to remove excessive formaldehyde.
Embodiment 2
A. the oleum 2100kg that 104.5% is put into the reaction kettle of 5000L, then heats to 120 DEG C, starts to delay
Slow that technical methylnaphthalene 2400kg is added dropwise, with the dropwise addition of technical methylnaphthalene, system temperature is gradually risen, and control dropping temperature is lower than
125 DEG C, drop finishes within about 3 hours, technical methylnaphthalene completion of dropwise addition, opens steam and is slowly warming up to 160 DEG C or so, while opening true
Sky maintains vacuum degree in 0.08MPa or so, insulation reaction 5h；
B. sulfonation terminates, and is cooled to 125 DEG C, 800kg water is slowly added dropwise, reaction is hydrolyzed, and hydrolysis terminates, and surveys acid value
21.94%；
C. hydrolysis terminates, and is discharged to condensation kettle, continues to be cooled to 75~80 DEG C, and the first that mass fraction is 37% is then added
Aldehyde 1000kg is finished and is to slowly warm up to 115 DEG C of progress condensation reaction 3h；
D. after condensation reaction, being neutralized to pH with liquid alkaline is 8.8, adds urea 200kg to remove excessive formaldehyde.
Embodiment 3
A. 98% sulfuric acid 2500kg is put into 5000L glassed steel reaction vessels, then heats to 60 DEG C, starts to be slowly added dropwise
Technical methylnaphthalene 2400kg, with the dropwise addition of technical methylnaphthalene, system temperature is gradually risen, and control dropping temperature is lower than 125 DEG C,
Drop finishes within about 3 hours, technical methylnaphthalene completion of dropwise addition, opens steam and is slowly warming up to 160 DEG C or so, while opening vacuum, maintains
Vacuum degree is in 0.08MPa or so, insulation reaction 5h；
B. sulfonation terminates, and is cooled to 125 DEG C, 800kg water is slowly added dropwise, reaction is hydrolyzed, and hydrolysis terminates, and surveys acid value
22.71%；
C. hydrolysis terminates, and is discharged to condensation kettle, continues to be cooled to 75~80 DEG C, and the first that mass fraction is 37% is then added
Aldehyde 1000kg is finished and is to slowly warm up to 115 DEG C of progress condensation reaction 3h；
D. after condensation reaction, being neutralized to pH with liquid alkaline is 6.0, and it is excessive to remove to add appropriate urea 200kg
Formaldehyde.
Comparative example 1
A. technical methylnaphthalene 2400kg is put into 5000L glassed steel reaction vessels, is warming up to 120 DEG C, is slowly added dropwise
104.5% oleum 1900kg, 145 DEG C of dropping temperature of control is hereinafter, drop Bi Kaiqi steam is slowly warming up to 160 DEG C of left sides
The right side, while vacuum is opened, maintain vacuum degree in 0.08MPa or so, insulation reaction 5h；
B. sulfonation terminates, and is cooled to 125 DEG C, 750kg water is slowly added dropwise, reaction is hydrolyzed, and hydrolysis terminates, and surveys acid value
22.55%；
C. hydrolysis terminates, and is discharged to condensation kettle, continues to be cooled to 75~80 DEG C, and the first that mass fraction is 37% is then added
Aldehyde 1000kg is finished and is to slowly warm up to 115 DEG C of progress condensation reaction 3h；
D. after condensation reaction, being neutralized to pH with liquid alkaline is 6.5, adds urea 200kg to remove excessive formaldehyde.
Comparative example 2
A. technical methylnaphthalene 2400kg is put into 5000L glassed steel reaction vessels, is warming up to 60 DEG C, is slowly added dropwise
104.5% oleum 2400kg, 125 DEG C of dropping temperature of control is hereinafter, drop Bi Kaiqi steam is slowly warming up to 160 DEG C of left sides
The right side, while vacuum is opened, maintain vacuum degree in 0.08MPa or so, insulation reaction 5h；
B. sulfonation terminates, and is cooled to 125 DEG C, 800kg water is slowly added dropwise, reaction is hydrolyzed, and hydrolysis terminates, and surveys acid value
22.35%；
C. hydrolysis terminates, and is discharged to condensation kettle, continues to be cooled to 75~80 DEG C, and the first that mass fraction is 37% is then added
Aldehyde 1000kg is finished and is to slowly warm up to 105 carry out condensation reaction 4h；
D. after condensation reaction, being neutralized to pH with liquid alkaline is 7.5, and it is excessive to remove to add appropriate urea 200kg
Formaldehyde.
Comparative example 3
The concentrated sulfuric acid 120g that methyl naphthalene 100g, 98% are put into the four-hole boiling flask of 500mL opens stirring and is to slowly warm up to
130 DEG C, insulation reaction 4 hours；Heat preservation terminates to be cooled to 95 DEG C, and 65g water is slowly added dropwise at 90~100 DEG C for control temperature, is added dropwise
It finishes, continues insulation reaction 30 minutes；Heat preservation terminates, and the formaldehyde 50g that mass fraction is 37% is added into flask, at 100 DEG C
Reaction 1 hour；Heat preservation terminates, and is cooled to 85 DEG C, and calcium chloride 20g, and insulation reaction 45 minutes are added；It keeps the temperature in end liquid alkaline
With to pH close to 5, adds calcium hydroxide and adjust pH to 8 or so；Neutralization terminates, and filters to obtain Dispersant MF solution.
Performance test
According to professional standard HG/T2499-2013, the dyestuff that embodiment 1-3 and comparative example 1-3 are prepared is dispersed
Agent MF carries out contamination test, and concrete outcome is as shown in table 1 below.
Wherein, standard of the whiteness value of cloth specimen as evaluation Dispersant MF contamination is directly measured using spectrophotometric color measurement instrument.
Table 1
As can be seen from Table 1, the embodiment of the present application 1-3 is that technical methylnaphthalene is added dropwise in sulfuric acid, by the contamination of table 1
Test is as can be seen that the contamination of embodiment 1-3 is excellent compared to comparative example 1-3.And in terms of whiteness, the embodiment of the present application
The whiteness of 1-3 is much higher than comparative example 1-3.
Specifically, the hybrid mode of comparative example 1 and comparative example 2 is that sulfuric acid is added dropwise in technical methylnaphthalene, from contamination
Property test as can be seen that the contamination grade of embodiment 1-3 is superior to comparative example 1 and comparative example 2；It can also from whiteness test
Out, the whiteness test result of embodiment 1-3 is superior to comparative example 1 and comparative example 2.
The hybrid mode of comparative example 3 is that sulfuric acid and technical methylnaphthalene are blended, from contamination test as can be seen that embodiment
The contamination grade of 1-3 is superior to comparative example 3；From whiteness test it can also be seen that the whiteness test result of embodiment 1-3 is equal
Better than comparative example 3.
The above embodiment of the present invention be only to clearly illustrate example of the present invention, and not be to the present invention
Embodiment restriction.For those of ordinary skill in the art, it can also make on the basis of the above description
Other various forms of variations or variation.There is no necessity and possibility to exhaust all the enbodiments.It is all of the invention
Made any modifications, equivalent replacements, and improvements etc., should be included in the protection of the claims in the present invention within spirit and principle
Within the scope of.
Claims (9)
1. a kind of preparation method of Dispersant MF, which comprises the following steps:
Mixing step: naphthalene series compound is added dropwise in sulfuric acid system, obtains mix products；
Sulfonation procedure: the mix products are subjected to insulation reaction, obtain sulfonated products；
Hydrolysing step: being added water in the sulfonated products, and reaction is hydrolyzed, obtains hydrolysate；
Condensation step: being added formaldehyde in the hydrolysate, carries out condensation reaction, obtains condensation product.
2. preparation method according to claim 1, which is characterized in that the temperature of the mixing step is 40 DEG C or more, excellent
It is selected as 40~125 DEG C；And/or
The concentration of the sulfuric acid is 98% or more, and preferred concentration is 98%~104.5%.
3. preparation method according to claim 1 or 2, which is characterized in that in the mixing step, the naphthalene series compound
Molar ratio with sulfuric acid is 1:1.1~1.6, preferably 1:1.3~1.6.
4. preparation method according to claim 1-3, which is characterized in that in the sulfonation procedure, the heat preservation
Reaction is carried out in the presence of steam；
And/or the temperature of the insulation reaction is 130~180 DEG C, the time of the insulation reaction is 3~5h.
5. preparation method according to claim 1-4, which is characterized in that in sulfonation procedure, kept the temperature
When reaction, while using vacuum dewatering technique to remove the water generated during insulation reaction；Preferably, the vacuum dehydration work
In skill, vacuum degree is 0.04MPa or more.
6. preparation method according to claim 1-5, which is characterized in that in the hydrolysing step, hydrolysis
Temperature be 115~130 DEG C, preferably 120~128 DEG C；And/or
After the hydrolysis, the acid value of hydrolysate is 20~25%, preferably 22~23%.
7. preparation method according to claim 1-6, which is characterized in that in the condensation step, produced in hydrolysis
Temperature when formaldehyde being added in object is 75~80 DEG C；The temperature of condensation reaction is 100~120 DEG C；And/or
The molar ratio of formaldehyde and naphthalene series compound is 0.7~0.8:1.
8. a kind of Dispersant MF, which is characterized in that the Dispersant MF passes through the described in any item preparation methods of claim 1-7
It is prepared；The whiteness of the Dispersant MF is 25 or more, preferably 25-40.
9. Dispersant MF according to claim 8, which is characterized in that the whiteness is that detection obtains by the following method
:
The cloth after drawing a design is taken, the whiteness value of the cloth specimen is measured using spectrophotometric color measurement instrument.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910605949.7A CN110256303A (en) | 2019-07-05 | 2019-07-05 | Dispersant MF and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910605949.7A CN110256303A (en) | 2019-07-05 | 2019-07-05 | Dispersant MF and preparation method thereof |
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| CN111689879A (en) * | 2020-06-03 | 2020-09-22 | 浙江五龙新材股份有限公司 | Clean production method of dispersing agent |
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Application publication date: 20190920 |