CN108795101A - A kind of kneading method prepares the preparation process and permanent violet of permanent violet - Google Patents
A kind of kneading method prepares the preparation process and permanent violet of permanent violet Download PDFInfo
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- CN108795101A CN108795101A CN201710407648.4A CN201710407648A CN108795101A CN 108795101 A CN108795101 A CN 108795101A CN 201710407648 A CN201710407648 A CN 201710407648A CN 108795101 A CN108795101 A CN 108795101A
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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
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B67/00—Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
- C09B67/0001—Post-treatment of organic pigments or dyes
- C09B67/0002—Grinding; Milling with solid grinding or milling assistants
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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
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B67/00—Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
- C09B67/0001—Post-treatment of organic pigments or dyes
- C09B67/0014—Influencing the physical properties by treatment with a liquid, e.g. solvents
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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
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B67/00—Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
- C09B67/006—Preparation of organic pigments
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Abstract
The invention discloses preparation processes and permanent violet that a kind of kneading method prepares permanent violet, including：By permanent violet crude product, sodium chloride, and, it is mediated in diethylene glycol input kneader, obtains mediating material, the grain size for mediating material is -220 mesh of 180 mesh；Material will be mediated and handle the kneading material after being cleaned by removal of impurities；Kneading material after removal of impurities is surface-treated, finished product permanent violet is obtained after drying.The particle of permanent violet is kneaded into the permanent violet of grain size 180m-200m using kneading method by preparation process.It is mediated in kneading process and mutually collides between the particle of material, rubs so that permanent violet is ground into thinner particle.Material is mediated simultaneously during being tossed, mediates and expects to be thrown to dissipate, and mediate material under the action of viscosity during mediating material decline flocks together from newly again, reciprocal progress successively.It mediates material to experienced " throw and dissipate " " aggregation " many times and then ensure solid purple uniform particle sizes, the colour stable of permanent violet, transparency is good.
Description
Technical field
The present invention relates to the technical field of the preparation method of permanent violet, more particularly to a kind of kneading method prepares the system of permanent violet
Standby technique and permanent violet.
Background technology
Permanent violet bright in color light, strong coloring force, resistance to migration and favorable dispersibility, not only acidproof, alkaline-resisting, solvent resistant, but also have
Fabulous fast light, heat-resisting, against weather, is widely used in coating, plastics, rubber, leather, ink, paint etc..Permanent violet with
Other organic pigments are the same, always with minuteness particle fractions distribution in coloring medium when application, the crystal form of pigment particles, shape
The physical factors such as shape, size and surface state can all influence the reflection, absorption and scattering of light, to influence coloured light, tinting strength, tinting power, screening
Lid power and dispersibility, while the performances such as the fast light, heat-resisting of it, weatherability can also be impacted.
Permanent violet crude product is blackish green powder, is a kind of crystal based on α types, alpha type crystal stability is poor, in addition crude product
Particle is big, thus, tinting strength, tinting power is low, should not be used as commercial pigments, it is necessary to carry out pigmentation processing, reduce its granule size, and make
It is converted into performance stabilization, strong coloring force, the β type crystal of bright in color light.Permanent violet pigmentation shown in the prior art is usually adopted
With sour dissolved method.Sour dissolved method (US4317908, US4804417) is to dissolve or be partially dissolved in the concentrated sulfuric acid by permanent violet crude product,
It is subsequently poured into a large amount of deionized waters, it is made to be precipitated with tiny alpha type crystal, then handled through solvent and be translated into stable β types
Crystal, while improving crystal surface morphology, you can the permanent violet finished product being had excellent performance.
However, the prior art is by sour dissolved method, the grain size of the crystal of the permanent violet finished product permanent violet finished product of preparation is smaller,
Permanent violet finished color stability is poor.
Invention content
The goal of the invention of the present invention is to provide the preparation process and permanent violet that a kind of kneading method prepares permanent violet, to solve
The problem of the colour stability difference for the permanent violet that existing permanent violet preparation process prepares, while the application preparation is forever solid
Purple dispersion performance is good, strong covering power, and good resistance is all had to soda acid and organic solvent.
According to an embodiment of the invention in a first aspect, providing the preparation process that a kind of kneading method prepares permanent violet, including：
By permanent violet crude product, sodium chloride, and, it is mediated in diethylene glycol input kneader, obtains mediating material, the kneading
The grain size of material is -220 mesh of 180 mesh；
The kneading is expected to handle the kneading material after being cleaned by removal of impurities；
Kneading material after the removal of impurities is surface-treated, finished product permanent violet is obtained after drying.
It is selectable, by the permanent violet crude product, sodium chloride, and, it mediates, is pinched in diethylene glycol input kneader
Closing the step foregoing description technique expected further includes：
Permanent violet raw material is put into ball milling 20 hours in horizontal ball mill, obtains permanent violet crude product.
Selectable, described the step of permanent violet raw material is put into ball milling 20 hours in horizontal ball mill, includes：
The jacket temperature of the horizontal ball mill maintains 35 DEG C -40 DEG C.
Selectable, the step of material that will mediate is handled by removal of impurities, kneading material after being cleaned, includes：
After high speed dispersion is expected in the kneading, squeezes into filter press and carry out removing salt treatment, obtain the kneading material after desalination；
Hydrochloric acid is added into the kneading material after the desalination, the kneading material after being acidified；
Kneading material after the acidification is squeezed into and carries out alkali cleaning in filter press, obtains neutral kneading material；
By the kneading material of the neutrality, the sieve for 200 mesh that are sieved after high speed dispersion, the kneading material after being cleaned.
It is selectable, the step of kneading material by after removal of impurities is surface-treated, finished product permanent violet is obtained after drying
Including：
By the kneading material after the removal of impurities, it is added red base D, nitrate, resin dispersion liquid, hydrochloric acid, and, deionized water
After mixing, mixture is obtained；
The mixture is transferred to the washing of filter press deionization, until the mixture conductivity is reduced to 500 west gates
Every meter of son, the mixture after being cleaned；
Mixture after the cleaning is subjected to drying and processing, obtains finished product permanent violet.
It is selectable, the kneading material by after removal of impurities, the red base D of addition, nitrate, resin dispersion liquid, hydrochloric acid, with
And deionized water is after mixing, the step of obtaining mixture includes：
Under conditions of 80 DEG C, by the kneading material after the removal of impurities, red base D heat preservations is added, hydrochloric acid is added after twenty minutes,
After ten minutes, nitrate is added in heat preservation, and resin dispersion liquid is added in heat preservation after 1.5 hours, deionized water is added, is warming up to 90 DEG C,
Heat preservation cools down after 1.5 hours, obtains mixture.
Optionally, the kneading material after the removal of impurities, the deionized water, the red base D, the hydrochloric acid, the nitric acid
The mass ratio of salt, the resin dispersion liquid is 640:10600:45:44:18:61.
Optionally, the mass ratio of the permanent violet crude product, the sodium chloride, the diethylene glycol is 90:600:145.
Optionally, the process of the kneading carries out under conditions of 80 DEG C -90 DEG C.
Described in the embodiment of the present application second aspect shows described in a kind of permanent violet that permanent violet is shown in the embodiment of the present application
Preparation process be prepared.
By above technical scheme it is found that the embodiment of the present application shows that a kind of kneading method prepares the preparation process and forever of permanent violet
Gu purple, the preparation process, including：By permanent violet crude product, sodium chloride, and, it mediates, obtains in diethylene glycol input kneader
Material is mediated, the grain size for mediating material is -220 mesh of 180 mesh；The kneading is expected to handle the kneading after being cleaned by removal of impurities
Material；Kneading material after the removal of impurities is surface-treated, finished product permanent violet is obtained after drying.System shown in the embodiment of the present application
The particle of permanent violet is kneaded into the permanent violet of grain size 180m-200m using kneading method by standby technique.Material is mediated in kneading process
It mutually collides, rub between particle (the kneading material particle includes permanent violet and sodium chloride particle) so that permanent violet is ground into
Thinner particle.Material is mediated simultaneously during being tossed, and kneading material, which is thrown, to be dissipated, and is mediated during expecting to decline in viscosity
The lower kneading material of effect is again from newly flocking together, reciprocal progress successively.Mediate " throw and dissipate " " aggregation " for expecting experienced many times
And then ensure that frictional force, impact force that all permanent violet crude products in kneading material are subject to are uniform, and then ensure finished product permanent violet
Uniform particle sizes, the colour stable of permanent violet, transparency are good.
Further, the embodiment of the present application adds sodium chloride in mediating material, it is known that the hardness of sodium chloride crystal is larger, sodium chloride
Solubility in diethylene glycol is smaller, therefore sodium chloride exists with tiny graininess in kneading is expected, adds in mediating material
Enter sodium chloride, can significantly increase the frictional force mediated between material, during mediating material ascending motion with tangential motion, rubs
Wiping power contributes to solid purple crude product to be ground into smaller particle, and then shortens the time mediated.
Further, diethylene glycol is added in kneading material in the embodiment of the present application.The diethylene glycol is thick to permanent violet
Product have certain dissolubility, and then ensure that the kneading material has certain viscosity, and mediating material and bonding helps to stir in bulk
The permanent violet crude product mediated in expecting is cut into smaller particle by paddle.
Description of the drawings
It in order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, below will be to institute in embodiment
Attached drawing to be used is needed to be briefly described, it should be apparent that, the accompanying drawings in the following description is only some implementations of the present invention
Example, for those of ordinary skill in the art, without creative efforts, can also obtain according to these attached drawings
Obtain other attached drawings.
Fig. 1 is that the flow chart that a kind of kneading method exemplified prepares the preparation process of permanent violet is preferably implemented according to one；
Specific implementation mode
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Whole description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other
Embodiment shall fall within the protection scope of the present invention.
The stream that a kind of kneading method exemplified prepares the preparation process of permanent violet is preferably implemented for the application one as shown in Figure 1
Cheng Tu, the technique include：
S101 is by permanent violet crude product, sodium chloride, and, it is mediated in diethylene glycol input kneader, obtains mediating material, it is described
The grain size for mediating material is -220 mesh of 180 mesh；
It is provided with high-speed rotating stirring slurry in kneader and mediates material along pulp surface tangential motion, simultaneously because the work of centrifugal force
With, it mediates material and is thrown upwards, after rising to certain height, due to gravity, mediate material and fall into pulp surface again, and
It is tossed.The combination of this ascending motion and tangential motion makes kneading material be practically at continuous screw movement state.
Since paddle rotating speed is very high, material movement velocity is mediated also quickly, quickly the moving particle for mediating material is (described to pinch
It includes permanent violet and sodium chloride particle to close material particle) between mutually collide, rub so that permanent violet is ground into thinner particle.
Material is mediated simultaneously during being tossed, material is mediated and is dissipated by throwing, is mediated during material declines and is mediated under the action of viscosity
Material flocks together from newly again, reciprocal progress successively.Material is mediated to experienced " throw and dissipate " " aggregation " many times and then ensure to pinch
Frictional force, the impact force that all permanent violet crude products in conjunction material are subject to are uniform, and then ensure the uniform particle sizes of finished product permanent violet, forever
Gu purple colour stable, transparency are good.
Meanwhile the embodiment of the present application adds sodium chloride in mediating material, it is known that the hardness of sodium chloride crystal is larger, and sodium chloride exists
Solubility in diethylene glycol is smaller, therefore sodium chloride exists with tiny graininess in mediating material, is added in mediating material
Sodium chloride can significantly increase the frictional force mediated between material, during mediating material ascending motion with tangential motion, friction
Power contributes to solid purple crude product to be ground into smaller particle, and then shortens the time mediated.
Diethylene glycol is added in kneading material in the embodiment of the present application.The diethylene glycol has centainly permanent violet crude product
Dissolubility, and then ensure that kneadings material has certain viscosity, mediating material and bonding contributes to agitating paddle will kneading in bulk
Permanent violet crude product in material cuts into smaller particle.
During kneading, it is RL nanoparticles that the crystal form of permanent violet crude product turns brilliant by α-nanoparticle.
After permanent violet turns brilliant, tinting strength, tinting power and the transparency can be improved, while pigment itself can also be kept excellent
Solvent resistance and fast light heat resistance.
S102 expects the kneading to handle the kneading material after being cleaned by removal of impurities；
It mediates and usually there are some impurity in material, the presence of impurity, which frequently can lead to mediate, expects to assemble, and in turn results in
Permanent violet granularity it is uneven, cause the granularity of permanent violet uneven.The application is at impurity of the embodiment to mediating material
Reason pinches the impurity in material with removal, and then ensures that the granularity of permanent violet is uneven.
It is worth noting that：The purpose that technique shown in the embodiment of the present application designs removal step after kneading step is walked exists
In since kneading process carries out in kneader, kneader is usually that metal material is made, therefore, during pinching
It is no lack of and introduces some metal impurities, due to the presence of metal impurities, it will to the conductivity rising for causing to mediate material, and then makes to pinch
The permanent violet closed in material is assembled, and causes the granularity of permanent violet uneven, influences the tinctorial yield of permanent violet, transparency and color
Stability.
The embodiment of the present application expects to carry out removal of impurities processing, mediates the impurity in material with removal, prevent from mediating in material to mediating
Permanent violet is assembled, and the stability of the tinctorial yield of permanent violet, transparency and color is influenced.
Kneading material after the removal of impurities is surface-treated by S103, and finished product permanent violet is obtained after drying.
In order to further prevent the aggregation of permanent violet, ensure that the particle of permanent violet is uniform,
The embodiment of the present application is surface-treated the kneading material after removal of impurities, to improve the dispersibility of the permanent violet, protects
The particle for demonstrate,proving permanent violet is uniform.So that finished product permanent violet colour stable, transparency is high.
It is selectable, by the permanent violet crude product, sodium chloride, and, it mediates, is pinched in diethylene glycol input kneader
Closing the step foregoing description technique expected further includes：
Permanent violet raw material is put into ball milling 20 hours in horizontal ball mill, obtains permanent violet crude product.
In order to shorten kneading time, permanent violet raw material is put into ball in horizontal ball mill by the embodiment of the present application before kneading
Mill 20 hours, obtains permanent violet crude product.
The embodiment of the present application needs the granularity for mediating the permanent violet in material forever being kneaded into -220 mesh of 180 mesh, if directly will
Permanent violet crude product, sodium chloride, and, it is mediated in diethylene glycol input kneader, needs to mediate 50h.
In order to shorten kneading time, reduce the consumption of electric energy, the embodiment of the present application " kneading " the step of before added one
The process of " grinding ".
Permanent violet raw material is put into ball milling 20 hours in horizontal ball mill, obtains permanent violet crude product；
There are some coarse particles for known permanent violet raw material middle, if directly by permanent violet raw material and diethylene glycol, chlorine
Change sodium mixing；Solubility of the permanent violet of some big particles in diethylene glycol is poor, at this point, the permanent violet of big particle exists
Viscosity is smaller during kneading, and therefore, the permanent violet of big particle no longer sticks to each other, but is individually present.In decline
In the process, the rate that the permanent violet of big particle declines is slower, therefore, reduces the efficiency of kneading.
Practice have shown that if directly by permanent violet raw material and diethylene glycol, sodium chloride mixing needs to mediate 50 hours, mediates material
In the granularity of permanent violet can reach -200 mesh of 180 mesh.
If permanent violet raw material is put into ball milling 20 hours in horizontal ball mill in advance, permanent violet crude product is obtained, it then will forever
Gu purple crude product and diethylene glycol, sodium chloride mixing need to mediate 6 hours, 180 can be reached by mediating the granularity of the permanent violet in material
- 200 mesh of mesh.
It can be seen that permanent violet raw material is put into ball milling 20 hours in horizontal ball mill in advance, permanent violet crude product is obtained, then will
Permanent violet crude product and sodium chloride are mediated after diethylene glycol mixing, can effectively shorten kneading time, improve the efficiency of kneading.
Selectable, described the step of permanent violet raw material is put into ball milling 20 hours in horizontal ball mill, includes：
The jacket temperature of the horizontal ball mill maintains 35 DEG C -40 DEG C.
The horizontal ball mill grinding that the embodiment of the present application uses is at low cost, and inventory is big, no benzene residual.It can grind every time
The permanent violet raw material of 700kg.
It is a physics temperature-rise period in process of lapping, permanent violet raw material will produce heat with steel-ball collision, and temperature increases,
Pressure in horizontal ball mill is caused to increase, so being ground under cooling environment.
The jacket temperature of horizontal ball mill is maintained 35 DEG C -40 DEG C by the embodiment of the present application, to prevent from producing in process of lapping
Raw hyperbaric environment.
Selectable, the step of material that will mediate is handled by removal of impurities, kneading material after being cleaned, includes：
After the kneading is expected high speed dispersion by S1021, squeezes into filter press and carry out removing salt treatment, obtain the kneading after desalination
Material；
It is worth noting that：After high speed dispersion is expected in the kneading, squeezes into filter press and carry out removing salt treatment, obtain desalination
Kneading material afterwards.The sodium chloride crystal that purpose is to mediate in material washes out.
Known sodium chloride is polar substances, and solubility in deionized water is larger, permanent violet in deionized water molten
Xie Du is smaller, and the embodiment of the present application is passed through a large amount of deionized water in filter press, and sodium chloride dissolves shape in deionized water at this time
At solution, permanent violet disperses in the form of granules with deionized water, and filtering detaches permanent violet with deionized water.
The embodiment of the present application recrystallizes the solution of sodium chloride, and sodium chloride is recycled.
Hydrochloric acid is added into the kneading material after the desalination in S1022, the kneading material after being acidified；
There may be the iron filings generated in collision due to steel ball, these remaining iron filings can lead to electricity during grinding
Conductance increases, and then increases the electrostatic force between permanent violet, and under the action of electrostatic attraction, permanent violet can be assembled, in turn
It causes the granularity of permanent violet uneven, influences the stability of the tinctorial yield of permanent violet, transparency and color.
Hydrochloric acid is added in mediating material in the embodiment of the present application, and the metal impurities in material are mediated with removal, reduces kneading material
Conductivity prevents permanent violet from assembling, and ensures permanent violet uniform particle sizes, and then ensure the colour stable of permanent violet, transparency
It is good.
The embodiment of the present application is deionized water and the concentration of hydrochloric acid.700kg permanent violet raw materials are added every time, in the mistake of pickling
The metal impurities in expecting can will be mediated in journey with 31% concentrated hydrochloric acid 387kg and 2613kg deionized water of content to remove.
Kneading material after the acidification is squeezed into and carries out alkali cleaning in filter press by S1023, obtains neutral kneading material；
Kneading material after acidification is squeezed into and carries out alkali cleaning in filter press by the embodiment of the present application, and the lye of generally use is carbonic acid
Hydrogen sodium solution, sodium carbonate liquor.To ensure the pH for mediating material at neutrality.
The content of hydrochloric acid in stringent control permanent violet is needed in subsequent surface treatment process.
Although the amount for the hydrochloric acid being added in this step is it is known that still, the amount of iron tramp is introduced in each production process
It is random.So can not accurately in control permanent violet remaining hydrochloric acid content.Therefore, I can not learn and subsequently need to be added
The amount of hydrochloric acid.
Although the surplus of hydrochloric acid, pH test paper and acidometer can be measured by pH test paper or acidometer
With the content of rough measurement hydrochloric acid, but it can not accurately obtain the surplus of hydrochloric acid.
In order to ensure being smoothed out for sequent surface processing procedure, ensure hydrochloric acid in stringent control surface treatment process plus
Enter amount.Kneading material after the acidification will be squeezed into and carries out alkali cleaning in filter press by the embodiment of the present application, obtain neutral kneading material.
S1024 is by the kneading material of the neutrality, the sieve for 200 mesh that are sieved after high speed dispersion, the kneading material after being cleaned.
It is no lack of during grinding and introduces some bigger iron blocks, hydrochloric acid is added at this time can not be molten by larger iron block
Solution.Meanwhile some sundries usually contained in sodium chloride, the presence of the kneader the inside larger impurity of volume is to permanent violet grain
The homogeneity of diameter generates certain influence.
The embodiment of the present application ensures the homogeneity of permanent violet grain size to further remove the impurity in permanent violet, will in
The kneading material of property, the sieve for 200 mesh that are sieved after high speed dispersion is to remove the impurity of some large volumes in permanent violet.
There may be the iron filings generated in collision due to steel ball, these remaining iron filings can lead to electricity during grinding
Conductance increases, and under the action of electrostatic attraction, permanent violet can occur aggregation and cause the granularity of permanent violet uneven, influences forever solid
The stability of purple tinctorial yield, transparency and color.
It is selectable, the step of kneading material by after removal of impurities is surface-treated, finished product permanent violet is obtained after drying
Including：
Red base D is added in kneading material after the removal of impurities by S1031, nitrate, resin dispersion liquid, hydrochloric acid, and, it goes
Ionized water after mixing, obtains mixture；
The embodiment of the present application surface treatment substance is added red base D, nitrate, resin dispersion liquid, hydrochloric acid, and, go from
Sub- water；
Wherein, the gorgeous degree for being designed to provide permanent violet of red base D is added；The purpose that resin dispersion liquid is added is to carry
The dispersibility of high permanent violet prevents the aggregation of permanent violet, improves the stability of permanent violet.
The purpose of nitrate is added in the viscosity for adjusting permanent violet, and then adjusts the mobility of permanent violet.Nitrate is added
Amount is more, and permanent violet viscosity is lower.
The mixture is transferred to the washing of filter press deionization by S1032, until the mixture conductivity is reduced to 500
Every meter of Siemens, the mixture after being cleaned；
Mixture is further washed with deionized water the application, to reduce mixture conductivity.
Mixture after the cleaning is carried out drying and processing by S1033, obtains finished product permanent violet.
It is selectable, the kneading material by after removal of impurities, the red base D of addition, nitrate, resin dispersion liquid, hydrochloric acid, with
And deionized water is after mixing, the step of obtaining mixture includes：
Under conditions of 80 DEG C, by the kneading material after the removal of impurities, red base D heat preservations is added, hydrochloric acid is added after twenty minutes,
After ten minutes, nitrate is added in heat preservation, and resin dispersion liquid is added in heat preservation after 1.5 hours, deionized water is added, is warming up to 90 DEG C,
Heat preservation cools down after 1.5 hours, obtains mixture.
In order to further increase the dispersibility of permanent violet, the embodiment of the present application is during surface treatment, first, 80
Under conditions of DEG C, by the kneading material after the removal of impurities, red base D heat preservations is added, hydrochloric acid is added after twenty minutes, to ensure addition
Red base D, hydrochloric acid are uniformly mixed with the kneading material after removal of impurities, and the mobility that nitrate adjusts permanent violet is added, is eventually adding tree
Fat dispersion liquid, deionized water further increase the dispersibility of permanent violet.
It is selectable, the deionized water, the red base D, the hydrochloric acid, the nitrate, the resin dispersion liquid
Mass ratio be 640:10600:45:44:18:61.
Wherein, nitrate is to adjust the mobility of permanent violet finished product and the covering power of finished product permanent violet, using the application
With preferable covering power while the finished product permanent violet that the ratio for implementing to exemplify is prepared is with good mobility.
The addition of resin dispersion liquid directly affects the stability of finished product permanent violet color.In a certain range with tree
The dispersibility of the increase of fat dispersion liquid addition, finished product permanent violet is better, and the stability of finished product permanent violet color is better.
But kneading material after removal of impurities is 640 with resin dispersion liquid mass ratio：61, even if follow-up continue growing resin point
The addition of dispersion liquid improves the dispersibility of the permanent violet of finished product without apparent.Resin dispersion liquid is continued growing at this time, it will drop
The covering power of low finished product permanent violet.
Selectable, the mass ratio of the permanent violet crude product, the sodium chloride, the diethylene glycol is 90:600:145.
The embodiment of the present application second aspect shows a kind of permanent violet, the colour stable of the permanent violet, and transparency is good.
By above technical scheme it is found that the embodiment of the present application shows that a kind of kneading method prepares the preparation process and forever of permanent violet
Gu purple, the preparation process, including：By permanent violet crude product, sodium chloride, and, it mediates, obtains in diethylene glycol input kneader
Material is mediated, the grain size for mediating material is -220 mesh of 180 mesh；The kneading is expected to handle the kneading after being cleaned by removal of impurities
Material；Kneading material after the removal of impurities is surface-treated, finished product permanent violet is obtained after drying.System shown in the embodiment of the present application
The particle of permanent violet is kneaded into the permanent violet of grain size 180m-200m using kneading method by standby technique.Material is mediated in kneading process
It mutually collides, rub between particle (the kneading material particle includes permanent violet and sodium chloride particle) so that permanent violet is ground into
Thinner particle.Material is mediated simultaneously during being tossed, and kneading material, which is thrown, to be dissipated, and is mediated during expecting to decline in viscosity
The lower kneading material of effect is again from newly flocking together, reciprocal progress successively.Mediate " throw and dissipate " " aggregation " for expecting experienced many times
And then ensure that frictional force, impact force that all permanent violet crude products in kneading material are subject to are uniform, and then ensure finished product permanent violet
Uniform particle sizes, the colour stable of permanent violet, transparency are good.
Further, the embodiment of the present application adds sodium chloride in mediating material, it is known that the hardness of sodium chloride crystal is larger, sodium chloride
Solubility in diethylene glycol is smaller, therefore sodium chloride exists with tiny graininess in kneading is expected, adds in mediating material
Enter sodium chloride, can significantly increase the frictional force mediated between material, during mediating material ascending motion with tangential motion, rubs
Wiping power contributes to solid purple crude product to be ground into smaller particle, and then shortens the time mediated.
Further, diethylene glycol is added in kneading material in the embodiment of the present application.The diethylene glycol is thick to permanent violet
Product have certain dissolubility, and then ensure that the kneading material has certain viscosity, and mediating material and bonding helps to stir in bulk
The permanent violet crude product mediated in expecting is cut into smaller particle by paddle.
Those skilled in the art after considering the specification and implementing the invention disclosed here, will readily occur to its of the present invention
Its embodiment.This application is intended to cover the present invention any variations, uses, or adaptations, these modifications, purposes or
Person's adaptive change follows the general principle of the present invention and includes undocumented common knowledge in the art of the invention
Or conventional techniques.The description and examples are only to be considered as illustrative, and true scope and spirit of the invention are by following
Claim is pointed out.
It should be understood that the invention is not limited in the precision architectures for being described above and being shown in the accompanying drawings, and
And various modifications and changes may be made without departing from the scope thereof.The scope of the present invention is limited only by the attached claims.
Claims (10)
1. a kind of kneading method prepares the preparation process of permanent violet, which is characterized in that including：
By permanent violet crude product, sodium chloride, and, it is mediated in diethylene glycol input kneader, obtains mediating material, the material of mediating
Grain size is -220 mesh of 180 mesh；
The kneading is expected to handle the kneading material after being cleaned by removal of impurities；
Kneading material after the removal of impurities is surface-treated, finished product permanent violet is obtained after drying.
2. preparation process according to claim 1, which is characterized in that by the permanent violet crude product, sodium chloride, and, two
It is mediated in ethylene glycol input kneader, the step foregoing description technique for obtaining mediating material further includes：
Permanent violet raw material is put into ball milling 20 hours in horizontal ball mill, obtains permanent violet crude product.
3. preparation process according to claim 2, which is characterized in that described to put into permanent violet raw material in horizontal ball mill
The step of ball milling 20 hours includes：
The jacket temperature of the horizontal ball mill maintains 35 DEG C -40 DEG C.
4. preparation process according to claim 1, which is characterized in that the material that will mediate is handled by removal of impurities, is removed
The step of kneading material after miscellaneous includes：
After high speed dispersion is expected in the kneading, squeezes into filter press and carry out removing salt treatment, obtain the kneading material after desalination；
Hydrochloric acid is added into the kneading material after the desalination, the kneading material after being acidified；
Kneading material after the acidification is squeezed into and carries out alkali cleaning in filter press, obtains neutral kneading material；
By the kneading material of the neutrality, the sieve for 200 mesh that are sieved after high speed dispersion, the kneading material after being cleaned.
5. preparation process according to claim 1, which is characterized in that the kneading material by after removal of impurities carries out at surface
Reason, the step of finished product permanent violet is obtained after drying include：
By the kneading material after the removal of impurities, it is added red base D, nitrate, resin dispersion liquid, hydrochloric acid, and, deionized water mixing
After uniformly, mixture is obtained；
The mixture is transferred to the washing of filter press deionization, until to be reduced to 500 Siemens every for the mixture conductivity
Rice, the mixture after being cleaned；
Mixture after the cleaning is subjected to drying and processing, obtains finished product permanent violet.
6. preparation process according to claim 5, which is characterized in that red base is added in the kneading material by after removal of impurities
D, nitrate, resin dispersion liquid, hydrochloric acid, and, after mixing, the step of obtaining mixture includes deionized water：
Under conditions of 80 DEG C, by the kneading material after the removal of impurities, red base D heat preservations is added, hydrochloric acid is added after twenty minutes, keep the temperature
After ten minutes, nitrate is added, resin dispersion liquid is added in heat preservation after 1.5 hours, deionized water is added, and is warming up to 90 DEG C, heat preservation
Cool down after 1.5 hours, obtains mixture.
7. preparation process according to claim 5, which is characterized in that the kneading material after the removal of impurities, the deionized water,
The mass ratio of the red base D, the hydrochloric acid, the nitrate, the resin dispersion liquid are 640:10600:45:44:18:
61。
8. preparation process according to claim 1, which is characterized in that the permanent violet crude product, the sodium chloride, described two
The mass ratio of ethylene glycol is 90:600:145.
9. preparation process according to claim 1, which is characterized in that condition of the process of the kneading at 80 DEG C -90 DEG C
Lower progress.
10. a kind of permanent violet, which is characterized in that the permanent violet is by preparation process system described in any one of claim 1-9
It is standby to form.
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| CN111847481A (en) * | 2020-08-27 | 2020-10-30 | 银川百泓新材料科技有限公司 | Method and device for recycling sodium chloride and diethylene glycol from permanent violet kneading wastewater |
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Application publication date: 20181113 |