CN106948214A - A kind of preparation method of attapulgite filler - Google Patents

A kind of preparation method of attapulgite filler Download PDF

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Publication number
CN106948214A
CN106948214A CN201710235699.3A CN201710235699A CN106948214A CN 106948214 A CN106948214 A CN 106948214A CN 201710235699 A CN201710235699 A CN 201710235699A CN 106948214 A CN106948214 A CN 106948214A
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attapulgite
parts
preparation
drying
filler
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李振国
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MINGGUANG GUOXING ATTAPULGITE CLAY Co Ltd
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MINGGUANG GUOXING ATTAPULGITE CLAY Co Ltd
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Priority to CN201710235699.3A priority Critical patent/CN106948214A/en
Publication of CN106948214A publication Critical patent/CN106948214A/en
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    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
    • D21H17/63—Inorganic compounds
    • D21H17/67—Water-insoluble compounds, e.g. fillers, pigments
    • D21H17/69—Water-insoluble compounds, e.g. fillers, pigments modified, e.g. by association with other compositions prior to incorporation in the pulp or paper
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
    • D21H17/63—Inorganic compounds
    • D21H17/67—Water-insoluble compounds, e.g. fillers, pigments
    • D21H17/68—Water-insoluble compounds, e.g. fillers, pigments siliceous, e.g. clays
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
    • D21H17/03—Non-macromolecular organic compounds
    • D21H17/05—Non-macromolecular organic compounds containing elements other than carbon and hydrogen only
    • D21H17/13—Silicon-containing compounds
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
    • D21H17/03—Non-macromolecular organic compounds
    • D21H17/05—Non-macromolecular organic compounds containing elements other than carbon and hydrogen only
    • D21H17/17—Ketenes, e.g. ketene dimers
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
    • D21H17/20—Macromolecular organic compounds
    • D21H17/21—Macromolecular organic compounds of natural origin; Derivatives thereof
    • D21H17/23—Lignins
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
    • D21H17/20—Macromolecular organic compounds
    • D21H17/21—Macromolecular organic compounds of natural origin; Derivatives thereof
    • D21H17/24—Polysaccharides
    • D21H17/25—Cellulose
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
    • D21H17/20—Macromolecular organic compounds
    • D21H17/21—Macromolecular organic compounds of natural origin; Derivatives thereof
    • D21H17/24—Polysaccharides
    • D21H17/30—Alginic acid or alginates
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
    • D21H17/20—Macromolecular organic compounds
    • D21H17/33—Synthetic macromolecular compounds
    • D21H17/46—Synthetic macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D21H17/47—Condensation polymers of aldehydes or ketones
    • D21H17/49—Condensation polymers of aldehydes or ketones with compounds containing hydrogen bound to nitrogen
    • D21H17/51—Triazines, e.g. melamine
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
    • D21H17/20—Macromolecular organic compounds
    • D21H17/33—Synthetic macromolecular compounds
    • D21H17/46—Synthetic macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D21H17/53—Polyethers; Polyesters
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
    • D21H17/60—Waxes
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
    • D21H17/63—Inorganic compounds
    • D21H17/66—Salts, e.g. alums

Abstract

The invention discloses a kind of preparation method of attapulgite filler, it is related to attapulgite technical field, including（1）, attapulgite pretreatment；（2）, attapulgite just finished product preparation；（3）, vapor modification；（4）, surface modification treatment；（5）, slurry prepare；（6）, spray drying.The present invention is using attapulgite as primary raw material.Modification twice is carried out to it and filler additive is added, it is possible to increase mothproof performance, intensity and the toughness of paper, resistance to writing, in addition, the attapulgite filler of the present invention prepares simple, is easy to preserve.

Description

A kind of preparation method of attapulgite filler
Technical field
The present invention relates to attapulgite technical field, and in particular to a kind of preparation method of attapulgite filler.
Background technology
Attapulgite has good colloidal nature and the higher adsorption bleachings such as unique scattered, high temperature resistant, salt resistance alkali Ability.And with certain plasticity and cohesive force, water imbibition is strong, has viscosity and plasticity when wet, dry after-contraction is small, less Aobvious crackle, water immersion disintegration, suspension meets dielectric not flocculation sediment.Therefore attapulgite is widely used in sewage disposal, suction The numerous areas such as attached purification, detergent, rubber, coating, papermaking, light industry, agricultural, cosmetics, are a kind of important nonmetallic ores Production.In order to further improve the using effect of attapulgite, strengthen its overall physical and chemical performance, generally it is entered using preceding Row modification, to improve the dispersive property of attapulgite, gel viscosity, colloidity, rheological property.Current modified attapulgite The need for soil can not meet production and living in many performances, in addition it is also necessary to further improve its performance.
In order to improve paper optical property and printability, fibrous raw material reduction production cost is saved, in the production of paper In, typically it is required to add filler.Because the price of general filler only has the 1/10th even lower of string price, because This, adds more fillers in paper, can significantly reduce paper production cost.Attapulgite is used as filler, performance It is excellent, but also due to particle diameter, the difference of surface topography, it is filled with rear paper properties and would also vary from, it is necessary to change to it Property, improve the performances such as its intensity, toughness.
The content of the invention
It is an object of the invention to provide a kind of preparation method of attapulgite filler, using attapulgite to be main former Material.Modification twice is carried out to it and filler additive is added, it is possible to increase mothproof performance, intensity and the toughness of paper, it is resistance to Writing, in addition, the attapulgite filler of the present invention prepares simple, is easy to preserve.
The invention provides following technical scheme：A kind of preparation method of attapulgite filler, including following step Suddenly：
（1）, attapulgite pretreatment：Take attapulgite to crush, granular size is crushed to for 18~28 mesh, in the situation of stirring Under, attapulgite is added in distilled water, solid-liquid weight ratio is 1:15~1：20, stirred at normal temperatures with 150~180 r/min After 2~2.5h, gained slurry is centrifuged off detrital mineral with centrifuge, attapulgite essence is obtained by filtering, drying steps Soil；
（2）, attapulgite just finished product preparation：By step（1）Obtain attapulgite essence soil be added to by a certain percentage from In sub- water, attapulgite suspension is made, filtering and standing obtains attapulgite just finished product after drying；
（3）, vapor modification：By step（2）In obtained attapulgite just finished product is increased to 300~320 DEG C from room temperature, And be passed through inert gas and make vapor and attapulgite haptoreaction, the reaction time is 1~1.5h, and reaction stops adding after terminating Vapor, after temperature is down to room temperature, takes out attapulgite, is washed and dry attapulgite modified semi-finished product；
（4）, surface modification treatment：Heating stepses（3）In obtain obtaining attapulgite modified semi-finished product, temperature control is 50~60 DEG C, add cationic surfactant under stirring, cationic surfactant quality account for attapulgite quality 2~ 10%, 15 ~ 20h of stirring reaction, add activation dispersant, stir, and filtering and standing obtains attapulgite modified after drying；
（5）, slurry prepare：By step（4）Obtained modified attapulgite rod soil adds quality in 20 ~ 30 times of clear water, stirring is equal It is even to obtain mixed slurry；
（6）, spray drying：To step（5）80 ~ 85 DEG C of hot-air is blown in obtained mixed slurry seethes it, then to seething Powder in spray into vaporific filler additive, make after the two is sufficiently mixed, keeping temperature is 75 ~ 85 DEG C, continue to seethe 20 ~ 25min, by vibrating-disk drying machine of the resulting material by tape transport to the basin containing multilayer, control drying temperature is 40 DEG C~45 DEG C, when drying materials to moisture content are less than 0.8%, material is delivered to disc flour mill, concave convex rod handmade paper is obtained Open filler.
Preferably, the step（2）Middle concave convex rod soil property amount accounts for the 2%~15% of ionized water gross mass.
Preferably, the step（3）Middle inert gas is nitrogen.
Preferably, the step（3）In vapor and nitrogen volume ratio be 1：（15~20）, vapor and concave convex rod Soil mass ratio be（60~100）：1.
Preferably, the step（4）Middle activation dispersant is stearic acid or Tissuemat E.
Preferably, the step（4）In cationic surfactant be organic ammonium salt.
Preferably, the organic ammonium salt be specially Cetyltrimethylammonium bromide, OTAC, Cetyl trimethylammonium bromide, hexadecyltrimethylammonium chloride, TTAB, tetradecyltrimethylammonium Ammonium chloride, DTAB, DTAC, dodecyl benzyl dimethyl ammonium chloride, ten Any of tetraalkyl dimethyl benzyl ammonium chloride.
Preferably, the step（6）In filler additive by weight include 20 ~ 30 parts of sodium alginate, anhydrous second 20 ~ 30 parts of alcohol, 20 ~ 30 parts of camphortree bark, 20 ~ 30 parts of folium artemisiae argyi, 10 ~ 15 parts of alkyl ketene dimer, 10 ~ 15 parts of solid paraffin, second 10 ~ 15 parts of alkenyl trimethoxy silane, 2 ~ 8 parts of nano-bentonite, 2 ~ 8 parts of sodium carbonate, 2 ~ 8 parts of styrene-butadiene emulsion, dryness alkyd tree 1 ~ 3 part of 2 ~ 8 parts of fat, 2 ~ 8 parts of melamine resin, 1 ~ 3 part of tourmaline powder, 1 ~ 3 part of microcrystalline cellulose and sodium laurate.
Preferably, the step（6）In spray-drying installation using high pressure draught drive material pass through spray nozzle, by thing Material is injected in the chamber of cyclone separator in the form of droplet particle, and dry air is passed through in cyclone separator.
Beneficial effects of the present invention：Using attapulgite as primary raw material.Modification twice is carried out to it and filler is added Additive, it is possible to increase mothproof performance, intensity and the toughness of paper, resistance to writing, in addition, the attapulgite filler of the present invention Prepare simple, be easy to preserve, it is specific as follows：
（1）, using water vapour to attapulgite carry out first time modification, the processing procedure pickling-free discharge of wastewater, improve The environmentally friendly efficiency of production process, because process shortens during water vapour modification, improves production efficiency, reduces life The vapor modification carried out under cost, proper temperature is produced, attapulgite's surface performance can be improved, its adsorption capacity is improved, Its application field is further widened, is significantly improved using the hydrophobicity of the modified attapulgite of this method；
（2）, addition folium artemisiae argyi and camphortree bark, the moth-proof and mould-proof performance for improving paper, in addition folium artemisiae argyi make paper that there is fragrance；
（3）, by the way of spray drying, be easy to filler to be preserved in the form of dried powder, the holding time is greatly prolonged, It is easy to use when configuring filler simultaneously, it is only necessary to which filler powder is dispersed in paper pulp.
Embodiment
With reference to specific embodiment, the present invention is expanded on further.These embodiments be merely to illustrate the present invention and without In limitation the scope of the present invention.
Embodiment 1
A kind of preparation method of attapulgite filler, comprises the following steps：
（1）, attapulgite pretreatment：Take attapulgite to crush, be crushed to granular size for 18 mesh, will in the case of stirring Attapulgite is added in distilled water, and solid-liquid weight ratio is 1:15, stirred at normal temperatures with 150 r/min after 2h, will with centrifuge Gained slurry is centrifuged off detrital mineral, and attapulgite essence soil is obtained by filtering, drying steps；
（2）, attapulgite just finished product preparation：By step（1）Obtain attapulgite essence soil be added to by a certain percentage from In sub- water, attapulgite suspension is made, filtering and standing obtains attapulgite just finished product after drying；
（3）, vapor modification：By step（2）In obtained attapulgite just finished product is increased to 300 DEG C from room temperature, and lead to Entering inert gas makes vapor and attapulgite haptoreaction, and the reaction time is 1h, and reaction stops adding vapor after terminating, and treats Temperature is down to after room temperature, takes out attapulgite, is washed and dry attapulgite modified semi-finished product；
（4）, surface modification treatment：Heating stepses（3）In obtain obtaining attapulgite modified semi-finished product, temperature control is 50 DEG C, Cationic surfactant is added under stirring, cationic surfactant quality accounts for the 2% of attapulgite quality, and stirring is anti- 15h is answered, activation dispersant is added, stirs, filtering and standing obtains attapulgite modified after drying；
（5）, slurry prepare：By step（4）Obtained modified attapulgite rod soil adds quality in 20 times of clear water, to stir To mixed slurry；
（6）, spray drying：To step（5）80 DEG C of hot-air is blown in obtained mixed slurry seethes it, then to the powder seethed Vaporific filler additive is sprayed into end, is made after the two is sufficiently mixed, keeping temperature is 75 DEG C, continues to seethe 20min, by gained Material controls drying temperature at 40 DEG C by the vibrating-disk drying machine of tape transport to the basin containing multilayer, treats that material dries Do to moisture content be less than 0.8% when, transfer the material into spray-drying installation, be described by the obtained powder of spray drying Attapulgite filler.
The step（2）Middle concave convex rod soil property amount accounts for the 2% of ionized water gross mass.
The step（3）Middle inert gas is nitrogen.
The step（3）In vapor and nitrogen volume ratio be 1：15, the mass ratio of vapor and attapulgite is 60：1.
The step（4）Middle activation dispersant is stearic acid.
The step（4）In cationic surfactant be organic ammonium salt.
The organic ammonium salt is Cetyltrimethylammonium bromide.
The step（6）In filler additive by weight include 20 parts of sodium alginate, 20 parts of absolute ethyl alcohol, camphor tree 20 parts of skin, 20 parts of folium artemisiae argyi, 10 parts of alkyl ketene dimer, 10 parts of solid paraffin, vinyltrimethoxy silane 10 part, nanometer are swollen 2 parts of profit soil, 2 parts of sodium carbonate, 2 parts of styrene-butadiene emulsion, 2 parts of dry alkyd resin, 2 parts of melamine resin, tourmaline powder 1 1 part of part, 1 part of microcrystalline cellulose and sodium laurate.
The step（6）In spray-drying installation using high pressure draught drive material pass through spray nozzle, by material with mist The form of drop particle is injected in the chamber of cyclone separator, and dry air is passed through in cyclone separator
Embodiment 2
A kind of preparation method of attapulgite filler, comprises the following steps：
（1）, attapulgite pretreatment：Take attapulgite to crush, be crushed to granular size for 28 mesh, will in the case of stirring Attapulgite is added in distilled water, and solid-liquid weight ratio is 1：20, stirred at normal temperatures with 180 r/min after 2.5h, use centrifuge Gained slurry is centrifuged off detrital mineral, attapulgite essence soil is obtained by filtering, drying steps；
（2）, attapulgite just finished product preparation：By step（1）Obtain attapulgite essence soil be added to by a certain percentage from In sub- water, attapulgite suspension is made, filtering and standing obtains attapulgite just finished product after drying；
（3）, vapor modification：By step（2）In obtained attapulgite just finished product is increased to 320 DEG C from room temperature, and lead to Entering inert gas makes vapor and attapulgite haptoreaction, and the reaction time is 1.5h, and reaction stops adding vapor after terminating, After temperature is down to room temperature, attapulgite is taken out, is washed and dry attapulgite modified semi-finished product；
（4）, surface modification treatment：Heating stepses（3）In obtain obtaining attapulgite modified semi-finished product, temperature control is 60 DEG C, Cationic surfactant is added under stirring, cationic surfactant quality accounts for the 10% of attapulgite quality, stirred 20h is reacted, activation dispersant is added, stirs, filtering and standing obtains attapulgite modified after drying；
（5）, slurry prepare：By step（4）Obtained modified attapulgite rod soil adds quality in 30 times of clear water, to stir To mixed slurry；
（6）, spray drying：To step（5）85 DEG C of hot-air is blown in obtained mixed slurry seethes it, then to the powder seethed Vaporific filler additive is sprayed into end, is made after the two is sufficiently mixed, keeping temperature is 85 DEG C, continues to seethe 25min, by gained Material controls drying temperature at 45 DEG C by the vibrating-disk drying machine of tape transport to the basin containing multilayer, treats that material dries Do to moisture content be less than 0.8% when, transfer the material into spray-drying installation, be described by the obtained powder of spray drying Attapulgite filler.
The step（2）Middle concave convex rod soil property amount accounts for the 15% of ionized water gross mass.
The step（3）Middle inert gas is nitrogen.
The step（3）In vapor and nitrogen volume ratio be 1：20, the mass ratio of vapor and attapulgite is 100：1.
The step（4）Middle activation dispersant is Tissuemat E.
The step（4）In cationic surfactant be organic ammonium salt.
The organic ammonium salt is OTAC.
The step（6）In filler additive by weight include 30 parts of sodium alginate, 30 parts of absolute ethyl alcohol, camphor tree 30 parts of skin, 30 parts of folium artemisiae argyi, 15 parts of alkyl ketene dimer, 15 parts of solid paraffin, vinyltrimethoxy silane 15 part, nanometer are swollen 8 parts of profit soil, 8 parts of sodium carbonate, 8 parts of styrene-butadiene emulsion, 8 parts of dry alkyd resin, 8 parts of melamine resin, tourmaline powder 3 3 parts of part, 3 parts of microcrystalline cellulose and sodium laurate.
The step（6）In spray-drying installation using high pressure draught drive material pass through spray nozzle, by material with mist The form of drop particle is injected in the chamber of cyclone separator, and dry air is passed through in cyclone separator
Embodiment 3
A kind of preparation method of attapulgite filler, comprises the following steps：
（1）, attapulgite pretreatment：Take attapulgite to crush, be crushed to granular size for 22 mesh, will in the case of stirring Attapulgite is added in distilled water, and solid-liquid weight ratio is 1:17, stirred at normal temperatures with 165 r/min after 2h, will with centrifuge Gained slurry is centrifuged off detrital mineral, and attapulgite essence soil is obtained by filtering, drying steps；
（2）, attapulgite just finished product preparation：By step（1）Obtain attapulgite essence soil be added to by a certain percentage from In sub- water, attapulgite suspension is made, filtering and standing obtains attapulgite just finished product after drying；
（3）, vapor modification：By step（2）In obtained attapulgite just finished product is increased to 310 DEG C from room temperature, and lead to Entering inert gas makes vapor and attapulgite haptoreaction, and the reaction time is 1h, and reaction stops adding vapor after terminating, and treats Temperature is down to after room temperature, takes out attapulgite, is washed and dry attapulgite modified semi-finished product；
（4）, surface modification treatment：Heating stepses（3）In obtain obtaining attapulgite modified semi-finished product, temperature control is 55 DEG C, Cationic surfactant is added under stirring, cationic surfactant quality accounts for the 7% of attapulgite quality, and stirring is anti- 17h is answered, activation dispersant is added, stirs, filtering and standing obtains attapulgite modified after drying；
（5）, slurry prepare：By step（4）Obtained modified attapulgite rod soil adds quality in 25 times of clear water, to stir To mixed slurry；
（6）, spray drying：To step（5）82 DEG C of hot-air is blown in obtained mixed slurry seethes it, then to the powder seethed Vaporific filler additive is sprayed into end, is made after the two is sufficiently mixed, keeping temperature is 80 DEG C, continues to seethe 22min, by gained Material controls drying temperature at 42 DEG C by the vibrating-disk drying machine of tape transport to the basin containing multilayer, treats that material dries Do to moisture content be less than 0.8% when, transfer the material into spray-drying installation, be described by the obtained powder of spray drying Attapulgite filler.
The step（2）Middle concave convex rod soil property amount accounts for the 8% of ionized water gross mass.
The step（3）Middle inert gas is nitrogen.
The step（3）In vapor and nitrogen volume ratio be 1：17, the mass ratio of vapor and attapulgite is 80：1.
The step（4）Middle activation dispersant is Tissuemat E.
The step（4）In cationic surfactant be organic ammonium salt.
The organic ammonium salt is DTAC.
The step（6）In filler additive by weight include 25 parts of sodium alginate, 25 parts of absolute ethyl alcohol, camphor tree 25 parts of skin, 25 parts of folium artemisiae argyi, 12 parts of alkyl ketene dimer, 12 parts of solid paraffin, vinyltrimethoxy silane 12 part, nanometer are swollen 6 parts of profit soil, 6 parts of sodium carbonate, 6 parts of styrene-butadiene emulsion, 6 parts of dry alkyd resin, 6 parts of melamine resin, tourmaline powder 2 2 parts of part, 2 parts of microcrystalline cellulose and sodium laurate.
The step（6）In spray-drying installation using high pressure draught drive material pass through spray nozzle, by material with mist The form of drop particle is injected in the chamber of cyclone separator, and dry air is passed through in cyclone separator
The present invention is described in detail with reference to the foregoing embodiments, for a person skilled in the art, it still may be used To be modified to the technical scheme described in foregoing embodiments, or to which part technical characteristic progress equivalent. Within the spirit and principles of the invention, any modifications, equivalent substitutions and improvements made etc., should be included in the present invention's Within protection domain.

Claims (9)

1. a kind of preparation method of attapulgite filler, it is characterised in that comprise the following steps：
（1）, attapulgite pretreatment：Take attapulgite to crush, granular size is crushed to for 18~28 mesh, in the situation of stirring Under, attapulgite is added in distilled water, solid-liquid weight ratio is 1:15~1：20, stirred at normal temperatures with 150~180 r/min After 2~2.5h, gained slurry is centrifuged off detrital mineral with centrifuge, attapulgite essence is obtained by filtering, drying steps Soil；
（2）, attapulgite just finished product preparation：By step（1）Obtain attapulgite essence soil be added to by a certain percentage from In sub- water, attapulgite suspension is made, filtering and standing obtains attapulgite just finished product after drying；
（3）, vapor modification：By step（2）In obtained attapulgite just finished product is increased to 300~320 DEG C from room temperature, And be passed through inert gas and make vapor and attapulgite haptoreaction, the reaction time is 1~1.5h, and reaction stops adding after terminating Vapor, after temperature is down to room temperature, takes out attapulgite, is washed and dry attapulgite modified semi-finished product；
（4）, surface modification treatment：Heating stepses（3）In obtain obtaining attapulgite modified semi-finished product, temperature control is 50~60 DEG C, add cationic surfactant under stirring, cationic surfactant quality account for attapulgite quality 2~ 10%, 15 ~ 20h of stirring reaction, add activation dispersant, stir, and filtering and standing obtains attapulgite modified after drying；
（5）, slurry prepare：By step（4）Obtained modified attapulgite rod soil adds quality in 20 ~ 30 times of clear water, stirring is equal It is even to obtain mixed slurry；
（6）, spray drying：To step（5）80 ~ 85 DEG C of hot-air is blown in obtained mixed slurry seethes it, then to seething Powder in spray into vaporific filler additive, make after the two is sufficiently mixed, keeping temperature is 75 ~ 85 DEG C, continue to seethe 20 ~ 25min, by vibrating-disk drying machine of the resulting material by tape transport to the basin containing multilayer, control drying temperature is 40 ~45 DEG C, when drying materials to moisture content are less than 0.8%, spray-drying installation is transferred the material into, is made by being spray-dried The powder obtained is the attapulgite filler.
2. the preparation method of attapulgite filler according to claim 1, it is characterised in that the step（2）In Attapulgite quality accounts for the 2~15% of ionized water gross mass.
3. the preparation method of attapulgite filler according to claim 1, it is characterised in that the step（3）In Inert gas is nitrogen.
4. the preparation method of attapulgite filler according to claim 3, it is characterised in that the step（3）In Vapor and nitrogen volume ratio be 1：（15~20）, the mass ratio of vapor and attapulgite is（60~100）：1.
5. the preparation method of attapulgite filler according to claim 1, it is characterised in that the step（4）In It is stearic acid or Tissuemat E to activate dispersant.
6. the preparation method of attapulgite filler according to claim 1, it is characterised in that the step（4）In Cationic surfactant be organic ammonium salt.
7. the preparation method of attapulgite filler according to claim 6, it is characterised in that the organic ammonium salt For Cetyltrimethylammonium bromide, OTAC, cetyl trimethylammonium bromide, cetyl front three Ammonium chloride, TTAB, tetradecyl trimethyl ammonium chloride, DTAB, 12 Any of alkyl trimethyl ammonium chloride, dodecyl benzyl dimethyl ammonium chloride, myristyl benzyl dimethyl ammonium chloride.
8. the preparation method of attapulgite filler according to claim 1, it is characterised in that the step（6）In Filler additive by weight include 20 ~ 30 parts of sodium alginate, 20 ~ 30 parts of absolute ethyl alcohol, 20 ~ 30 parts of camphortree bark, folium artemisiae argyi 20 ~ 30 parts, 10 ~ 15 parts of alkyl ketene dimer, 10 ~ 15 parts of solid paraffin, vinyltrimethoxy silane 10 ~ 15 part, nanometer 2 ~ 8 parts of bentonite, 2 ~ 8 parts of sodium carbonate, 2 ~ 8 parts of styrene-butadiene emulsion, 2 ~ 8 parts of dry alkyd resin, melamine resin 2 ~ 8 1 ~ 3 part of part, 1 ~ 3 part of tourmaline powder, 1 ~ 3 part of microcrystalline cellulose and sodium laurate.
9. the preparation method of attapulgite filler according to claim 1, it is characterised in that the step（6）In Spray-drying installation using high pressure draught drive material pass through spray nozzle, material is injected to whirlwind in the form of droplet particle Dry air is passed through in the chamber of separator, in cyclone separator.
CN201710235699.3A 2017-04-12 2017-04-12 A kind of preparation method of attapulgite filler Pending CN106948214A (en)

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Application publication date: 20170714