CN105419398A - Preparation method of Chinese prickly ash seed fatty acid modified heavy calcium carbonate - Google Patents

Preparation method of Chinese prickly ash seed fatty acid modified heavy calcium carbonate Download PDF

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CN105419398A
CN105419398A CN201510951411.3A CN201510951411A CN105419398A CN 105419398 A CN105419398 A CN 105419398A CN 201510951411 A CN201510951411 A CN 201510951411A CN 105419398 A CN105419398 A CN 105419398A
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water
calcium carbonate
fatty acid
ground limestone
heavy calcium
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仇颖超
林大伟
张帆
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/02Compounds of alkaline earth metals or magnesium
    • C09C1/021Calcium carbonates
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/08Treatment with low-molecular-weight non-polymer organic compounds
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40Additives
    • C09D7/60Additives non-macromolecular
    • C09D7/61Additives non-macromolecular inorganic
    • C09D7/62Additives non-macromolecular inorganic modified by treatment with other compounds

Abstract

The invention discloses a preparation method of Chinese prickly ash seed fatty acid modified heavy calcium carbonate and belongs to the technical field of preparation of calcium carbonate. According to the preparation method provided by the invention, by extracting fatty acid from Chinese prickly ash seed oil to modify heavy calcium carbonate, the surface property of the heavy calcium carbonate is changed, and the heavy calcium carbonate has better compatibility with organic high polymers, so that the Chinese prickly ash seed fatty acid modified heavy calcium carbonate is obtained. The embodiment proves that the operation is simple and feasible and raw materials are simple and easy to obtain; the defect that conventional heavy calcium carbonate has poor compatibility with the organic high polymers can be overcome; the application performance of a heavy calcium carbonate product is improved through modification.

Description

The preparation method of the fatty acid modified water-ground limestone of a kind of Semen Pericarpium Zanthoxyli
Technical field
The invention discloses the preparation method of the fatty acid modified water-ground limestone of a kind of Semen Pericarpium Zanthoxyli, belong to calcium carbonate preparing technical field.
Background technology
Water-ground limestone, also referred to as " coarse whiting ", is typically used as filler, is as calcite, marble, Wingdale grind and form by natural carbonate mineral.Be widely used in the industries such as rubber, plastics, papermaking, coating, cable, building product, food, medicine, weaving, play the volume increasing product as weighting agent, reduce production cost.
The technological process of production of current water-ground limestone has two kinds, is respectively dry technology for production flow process and wet process technique flow process.Wherein dry technology for production flow process refers to calcite, Wingdale, chalk, shell etc. that first picking is shipped from stone quarry, to remove gangue, then with crusher, coarse breaking is carried out to Wingdale, cover that (pendulum-type) abrasive dust is broken obtains microlith limestone flour again with thunder, finally carry out classification with grading machine to abrasive dust, the powder meeting granularity requirements is put in storage as the packing of product, otherwise returns pulverizing mill abrasive dust again, the method operation more complicated, cost compare is high; Other wet process technique flow process refers to that first dry method fine powder being made suspension is placed in grinding machine and pulverizes further, just superfine heavy calcium carbonate is obtained after dehydration, drying, although the method operation is more simple to operate than dry method, but the water-ground limestone particle very easily secondary agglomeration made, bad dispersibility, affects the application performance of product.
Summary of the invention
The technical problem that the present invention mainly solves: for current water-ground limestone in the process of producing, dry production operation more complicated, cost is high, and although the operating process of dry method complexity has been broken away from wet production operation, but have that bad dispersibility, particle are very easily agglomerating, the present situation of poor compatibility, provide one, by extracting lipid acid from Fructus Zanthoxyli oil, modification is carried out to water-ground limestone, change water-ground limestone surface properties, make itself and organic polymer have the method for better consistency.Operation is simple for the method, both solved the defect of conventional water-ground limestone and organic polymer poor compatibility, again by modification, improves the application performance of water-ground limestone product.
In order to solve the problems of the technologies described above, the technical solution adopted in the present invention is:
(1) take 4 ~ 5kg Semen Pericarpium Zanthoxyli and put into pot, after roasting 30 ~ 40min, after naturally cooling to room temperature, after wrapping with bundle, under putting into the pressing plate of high-pressure extrusion machine, suppress with the pressure of 0.2 ~ 0.3MPa, collect the Fructus Zanthoxyli oil squeezed out;
(2) measuring the Fructus Zanthoxyli oil that the above-mentioned compacting of 200 ~ 300mL obtains loads in the four-hole boiling flask of 500mL with agitator, reflux dropping funnel and thermometer, add the sodium hydroxide solution that 30 ~ 50mL concentration is 1mol/L inwards, start agitator and stir 10 ~ 20min with the rotating speed of 300 ~ 400r/min;
(3) be the ethanolic soln that 1:4 dropwise drips that in flask mass concentration is 75% by ethanol and Fructus Zanthoxyli oil volume ratio after stirring, move in water-bath, be heated to 60 ~ 70 DEG C, vibration 30 ~ 40min on shaking table is placed on after back flow reaction 1 ~ 2h, move in the ice-water bath of 4 ~ 6 DEG C again, leave standstill cooling 9 ~ 12h, saponification resultant is separated out completely;
(4) mixed solution of separating out saponification resultant is moved into Büchner funnel, after suction filtration removes ethanol, saponification resultant being dissolved in 200 ~ 300mL temperature is in the hot water of 50 ~ 70 DEG C, pH to 3 ~ 4 are regulated with the hydrochloric acid soln of 0.02mol/L, finally by mixed solution by being equipped with the funnel of sodium sulphite anhydrous 99.3, be separated obtain Fructus Zanthoxyli oil lipid acid;
(5) maleic anhydride of Fructus Zanthoxyli oil lipid acid obtained above for 0.05mol and 0.10mol is joined in the flask with agitator, add 50 ~ 60mL toluene and 20 ~ 30mL mass concentration is the toluenesulphonic acids of 10%, start agitator stir with the rotating speed of 400 ~ 500r/min and be warming up to 80 ~ 90 DEG C, isothermal reaction 7 ~ 9h; (6) reaction terminates rear deionized water wash mixed solution collection oil phase, oil phase is placed in rotatory evaporator, revolves boil off except toluene with the temperature of 50 ~ 60 DEG C, obtain tawny clear viscous liquid;
(7) 300 ~ 500g water-ground limestone is taken first with magnetic stirrer mechanical stirring activation 10 ~ 15min, measuring the above-mentioned obtained tawny clear viscous liquid of 100 ~ 200mL is again dissolved in 500 ~ 600mL dehydrated alcohol, mixed solution is sprayed in the water-ground limestone in high-speed stirring by high pressure spray nozzle, stirring velocity is 1000 ~ 1200r/min, finally put into thermostat container, discharging after insulated and stirred 30 ~ 40min at 90 ~ 100 DEG C, after cooling, namely packaging obtains the fatty acid modified water-ground limestone of a kind of Semen Pericarpium Zanthoxyli.
Application method of the present invention is: in the process making water-borne coatings, add the fatty acid modified water-ground limestone of Semen Pericarpium Zanthoxyli that water-borne coatings quality 20 ~ 50% the present invention obtains, as weighting agent, stir 3 ~ 5min with the rotating speed of 150 ~ 180r/min, it is made to mix completely.After testing, can find, with the addition of the coating not sedimentation of the fatty acid modified water-ground limestone of Semen Pericarpium Zanthoxyli that the present invention obtains, easily dispersion, glossiness is also good than the coating not adding the fatty acid modified water-ground limestone of Semen Pericarpium Zanthoxyli.
The invention has the beneficial effects as follows:
(1) production technique of the present invention is comparatively simple, and production cost is lower;
(2) the present invention is by rational technique, not only solves the defect of conventional water-ground limestone and organic polymer poor compatibility, and by modification, improves the application performance of water-ground limestone product.
Embodiment
First take 4 ~ 5kg Semen Pericarpium Zanthoxyli and put into pot, after roasting 30 ~ 40min, after naturally cooling to room temperature, after wrapping with bundle, under putting into the pressing plate of high-pressure extrusion machine, suppress with the pressure of 0.2 ~ 0.3MPa, collect the Fructus Zanthoxyli oil squeezed out; Then measuring the Fructus Zanthoxyli oil that the above-mentioned compacting of 200 ~ 300mL obtains loads in the four-hole boiling flask of 500mL with agitator, reflux dropping funnel and thermometer, add the sodium hydroxide solution that 30 ~ 50mL concentration is 1mol/L inwards, start agitator and stir 10 ~ 20min with the rotating speed of 300 ~ 400r/min; Be the ethanolic soln that 1:4 dropwise drips that in flask mass concentration is 75% by ethanol and Fructus Zanthoxyli oil volume ratio after stirring subsequently, move in water-bath, be heated to 60 ~ 70 DEG C, vibration 30 ~ 40min on shaking table is placed on after back flow reaction 1 ~ 2h, move in the ice-water bath of 4 ~ 6 DEG C again, leave standstill cooling 9 ~ 12h, saponification resultant is separated out completely; The mixed solution of separating out saponification resultant is moved into Büchner funnel, after suction filtration removes ethanol, saponification resultant being dissolved in 200 ~ 300mL temperature is in the hot water of 50 ~ 70 DEG C, pH to 3 ~ 4 are regulated with the hydrochloric acid soln of 0.02mol/L, finally by mixed solution by being equipped with the funnel of sodium sulphite anhydrous 99.3, be separated obtain Fructus Zanthoxyli oil lipid acid; Next the maleic anhydride of Fructus Zanthoxyli oil lipid acid obtained above for 0.05mol and 0.10mol is joined in the flask with agitator, add 50 ~ 60mL toluene and 20 ~ 30mL mass concentration is the toluenesulphonic acids of 10%, start agitator stir with the rotating speed of 400 ~ 500r/min and be warming up to 80 ~ 90 DEG C, isothermal reaction 7 ~ 9h; Reaction terminates rear deionized water wash mixed solution and collects oil phase, oil phase is placed in rotatory evaporator, revolves boil off except toluene with the temperature of 50 ~ 60 DEG C, obtain tawny clear viscous liquid; Finally take 300 ~ 500g water-ground limestone first with magnetic stirrer mechanical stirring activation 10 ~ 15min, measuring the above-mentioned obtained tawny clear viscous liquid of 100 ~ 200mL is again dissolved in 500 ~ 600mL dehydrated alcohol, mixed solution is sprayed in the water-ground limestone in high-speed stirring by high pressure spray nozzle, stirring velocity is 1000 ~ 1200r/min, finally put into thermostat container, discharging after insulated and stirred 30 ~ 40min at 90 ~ 100 DEG C, after cooling, namely packaging obtains the fatty acid modified water-ground limestone of a kind of Semen Pericarpium Zanthoxyli.
Example 1
First take 4kg Semen Pericarpium Zanthoxyli and put into pot, after roasting 30min, after naturally cooling to room temperature, after wrapping with bundle, under putting into the pressing plate of high-pressure extrusion machine, suppress with the pressure of 0.2MPa, collect the Fructus Zanthoxyli oil squeezed out; Then measuring the Fructus Zanthoxyli oil that the above-mentioned compacting of 200mL obtains loads in the four-hole boiling flask of 500mL with agitator, reflux dropping funnel and thermometer, add the sodium hydroxide solution that 30mL concentration is 1mol/L inwards, start agitator and stir 10min with the rotating speed of 300r/min; Be the ethanolic soln that 1:4 dropwise drips that in flask mass concentration is 75% by ethanol and Fructus Zanthoxyli oil volume ratio after stirring subsequently, move in water-bath, be heated to 60 DEG C, 30min that shaking table vibrates is placed on after back flow reaction 1h, move in the ice-water bath of 4 DEG C again, leave standstill cooling 9h, saponification resultant is separated out completely; The mixed solution of separating out saponification resultant is moved into Büchner funnel, after suction filtration removes ethanol, saponification resultant being dissolved in 200mL temperature is in the hot water of 50 DEG C, pH to 3 is regulated with the hydrochloric acid soln of 0.02mol/L, finally by mixed solution by being equipped with the funnel of sodium sulphite anhydrous 99.3, be separated obtain Fructus Zanthoxyli oil lipid acid; Next the maleic anhydride of Fructus Zanthoxyli oil lipid acid obtained above for 0.05mol and 0.10mol is joined in the flask with agitator, add 50mL toluene and 20mL mass concentration is the toluenesulphonic acids of 10%, start agitator stir with the rotating speed of 400r/min and be warming up to 80 DEG C, isothermal reaction 7h; Reaction terminates rear deionized water wash mixed solution and collects oil phase, oil phase is placed in rotatory evaporator, revolves boil off except toluene with the temperature of 50 DEG C, obtain tawny clear viscous liquid; Finally take 300g water-ground limestone first with magnetic stirrer mechanical stirring activation 10min, measuring the above-mentioned obtained tawny clear viscous liquid of 100mL is again dissolved in 500mL dehydrated alcohol, mixed solution is sprayed in the water-ground limestone in high-speed stirring by high pressure spray nozzle, stirring velocity is 1000r/min, finally put into thermostat container, discharging after insulated and stirred 30min at 90 DEG C, after cooling, namely packaging obtains the fatty acid modified water-ground limestone of a kind of Semen Pericarpium Zanthoxyli.
This example operation is simple, in the process making water-borne coatings, adds the fatty acid modified water-ground limestone of Semen Pericarpium Zanthoxyli that water-borne coatings quality 20% the present invention obtains, as weighting agent, stir 3min with the rotating speed of 150r/min, make it mix completely.After testing, can find, with the addition of the coating not sedimentation of the fatty acid modified water-ground limestone of Semen Pericarpium Zanthoxyli that the present invention obtains, easily dispersion, glossiness is also good than the coating not adding the fatty acid modified water-ground limestone of Semen Pericarpium Zanthoxyli.
Example 2
First take 4.5kg Semen Pericarpium Zanthoxyli and put into pot, after roasting 35min, after naturally cooling to room temperature, after wrapping with bundle, under putting into the pressing plate of high-pressure extrusion machine, suppress with the pressure of 0.25MPa, collect the Fructus Zanthoxyli oil squeezed out; Then measuring the Fructus Zanthoxyli oil that the above-mentioned compacting of 250mL obtains loads in the four-hole boiling flask of 500mL with agitator, reflux dropping funnel and thermometer, add the sodium hydroxide solution that 40mL concentration is 1mol/L inwards, start agitator and stir 15min with the rotating speed of 350r/min; Be the ethanolic soln that 1:4 dropwise drips that in flask mass concentration is 75% by ethanol and Fructus Zanthoxyli oil volume ratio after stirring subsequently, move in water-bath, be heated to 65 DEG C, 35min that shaking table vibrates is placed on after back flow reaction 1.5h, move in the ice-water bath of 5 DEG C again, leave standstill cooling 10h, saponification resultant is separated out completely; The mixed solution of separating out saponification resultant is moved into Büchner funnel, after suction filtration removes ethanol, saponification resultant being dissolved in 250mL temperature is in the hot water of 60 DEG C, pH to 3.5 is regulated with the hydrochloric acid soln of 0.02mol/L, finally by mixed solution by being equipped with the funnel of sodium sulphite anhydrous 99.3, be separated obtain Fructus Zanthoxyli oil lipid acid; Next the maleic anhydride of Fructus Zanthoxyli oil lipid acid obtained above for 0.05mol and 0.10mol is joined in the flask with agitator, add 55mL toluene and 25mL mass concentration is the toluenesulphonic acids of 10%, start agitator stir with the rotating speed of 450r/min and be warming up to 85 DEG C, isothermal reaction 8h; Reaction terminates rear deionized water wash mixed solution and collects oil phase, oil phase is placed in rotatory evaporator, revolves boil off except toluene with the temperature of 55 DEG C, obtain tawny clear viscous liquid; Finally take 400g water-ground limestone first with magnetic stirrer mechanical stirring activation 13min, measuring the above-mentioned obtained tawny clear viscous liquid of 150mL is again dissolved in 550mL dehydrated alcohol, mixed solution is sprayed in the water-ground limestone in high-speed stirring by high pressure spray nozzle, stirring velocity is 1100r/min, finally put into thermostat container, discharging after insulated and stirred 35min at 95 DEG C, after cooling, namely packaging obtains the fatty acid modified water-ground limestone of a kind of Semen Pericarpium Zanthoxyli.
This example operation is simple, in the process making water-borne coatings, adds the fatty acid modified water-ground limestone of Semen Pericarpium Zanthoxyli that water-borne coatings quality 40% the present invention obtains, as weighting agent, stir 4min with the rotating speed of 160r/min, make it mix completely.After testing, can find, with the addition of the coating not sedimentation of the fatty acid modified water-ground limestone of Semen Pericarpium Zanthoxyli that the present invention obtains, easily dispersion, glossiness is also good than the coating not adding the fatty acid modified water-ground limestone of Semen Pericarpium Zanthoxyli.
Example 3
First take 5kg Semen Pericarpium Zanthoxyli and put into pot, after roasting 40min, after naturally cooling to room temperature, after wrapping with bundle, under putting into the pressing plate of high-pressure extrusion machine, suppress with the pressure of 0.3MPa, collect the Fructus Zanthoxyli oil squeezed out; Then measuring the Fructus Zanthoxyli oil that the above-mentioned compacting of 300mL obtains loads in the four-hole boiling flask of 500mL with agitator, reflux dropping funnel and thermometer, add the sodium hydroxide solution that 50mL concentration is 1mol/L inwards, start agitator and stir 20min with the rotating speed of 400r/min; Be the ethanolic soln that 1:4 dropwise drips that in flask mass concentration is 75% by ethanol and Fructus Zanthoxyli oil volume ratio after stirring subsequently, move in water-bath, be heated to 70 DEG C, 40min that shaking table vibrates is placed on after back flow reaction 2h, move in the ice-water bath of 6 DEG C again, leave standstill cooling 12h, saponification resultant is separated out completely; The mixed solution of separating out saponification resultant is moved into Büchner funnel, after suction filtration removes ethanol, saponification resultant being dissolved in 300mL temperature is in the hot water of 70 DEG C, pH to 4 is regulated with the hydrochloric acid soln of 0.02mol/L, finally by mixed solution by being equipped with the funnel of sodium sulphite anhydrous 99.3, be separated obtain Fructus Zanthoxyli oil lipid acid; Next the maleic anhydride of Fructus Zanthoxyli oil lipid acid obtained above for 0.05mol and 0.10mol is joined in the flask with agitator, add 60mL toluene and 30mL mass concentration is the toluenesulphonic acids of 10%, start agitator stir with the rotating speed of 500r/min and be warming up to 90 DEG C, isothermal reaction 9h; Reaction terminates rear deionized water wash mixed solution and collects oil phase, oil phase is placed in rotatory evaporator, revolves boil off except toluene with the temperature of 60 DEG C, obtain tawny clear viscous liquid; Finally take 500g water-ground limestone first with magnetic stirrer mechanical stirring activation 15min, measuring the above-mentioned obtained tawny clear viscous liquid of 200mL is again dissolved in 600mL dehydrated alcohol, mixed solution is sprayed in the water-ground limestone in high-speed stirring by high pressure spray nozzle, stirring velocity is 1200r/min, finally put into thermostat container, discharging after insulated and stirred 40min at 100 DEG C, after cooling, namely packaging obtains the fatty acid modified water-ground limestone of a kind of Semen Pericarpium Zanthoxyli.
This example operation is simple, in the process making water-borne coatings, adds the fatty acid modified water-ground limestone of Semen Pericarpium Zanthoxyli that water-borne coatings quality 50% the present invention obtains, as weighting agent, stir 5min with the rotating speed of 180r/min, make it mix completely.After testing, can find, with the addition of the coating not sedimentation of the fatty acid modified water-ground limestone of Semen Pericarpium Zanthoxyli that the present invention obtains, easily dispersion, glossiness is also good than the coating not adding the fatty acid modified water-ground limestone of Semen Pericarpium Zanthoxyli.

Claims (1)

1. a preparation method for the fatty acid modified water-ground limestone of Semen Pericarpium Zanthoxyli, is characterized in that concrete preparation process is:
(1) take 4 ~ 5kg Semen Pericarpium Zanthoxyli and put into pot, after roasting 30 ~ 40min, after naturally cooling to room temperature, after wrapping with bundle, under putting into the pressing plate of high-pressure extrusion machine, suppress with the pressure of 0.2 ~ 0.3MPa, collect the Fructus Zanthoxyli oil squeezed out;
(2) measuring the Fructus Zanthoxyli oil that the above-mentioned compacting of 200 ~ 300mL obtains loads in the four-hole boiling flask of 500mL with agitator, reflux dropping funnel and thermometer, add the sodium hydroxide solution that 30 ~ 50mL concentration is 1mol/L inwards, start agitator and stir 10 ~ 20min with the rotating speed of 300 ~ 400r/min;
(3) be the ethanolic soln that 1:4 dropwise drips that in flask mass concentration is 75% by ethanol and Fructus Zanthoxyli oil volume ratio after stirring, move in water-bath, be heated to 60 ~ 70 DEG C, vibration 30 ~ 40min on shaking table is placed on after back flow reaction 1 ~ 2h, move in the ice-water bath of 4 ~ 6 DEG C again, leave standstill cooling 9 ~ 12h, saponification resultant is separated out completely;
(4) mixed solution of separating out saponification resultant is moved into Büchner funnel, after suction filtration removes ethanol, saponification resultant being dissolved in 200 ~ 300mL temperature is in the hot water of 50 ~ 70 DEG C, pH to 3 ~ 4 are regulated with the hydrochloric acid soln of 0.02mol/L, finally by mixed solution by being equipped with the funnel of sodium sulphite anhydrous 99.3, be separated obtain Fructus Zanthoxyli oil lipid acid;
(5) maleic anhydride of Fructus Zanthoxyli oil lipid acid obtained above for 0.05mol and 0.10mol is joined in the flask with agitator, add 50 ~ 60mL toluene and 20 ~ 30mL mass concentration is the toluenesulphonic acids of 10%, start agitator stir with the rotating speed of 400 ~ 500r/min and be warming up to 80 ~ 90 DEG C, isothermal reaction 7 ~ 9h; (6) reaction terminates rear deionized water wash mixed solution collection oil phase, oil phase is placed in rotatory evaporator, revolves boil off except toluene with the temperature of 50 ~ 60 DEG C, obtain tawny clear viscous liquid;
(7) 300 ~ 500g water-ground limestone is taken first with magnetic stirrer mechanical stirring activation 10 ~ 15min, measuring the above-mentioned obtained tawny clear viscous liquid of 100 ~ 200mL is again dissolved in 500 ~ 600mL dehydrated alcohol, mixed solution is sprayed in the water-ground limestone in high-speed stirring by high pressure spray nozzle, stirring velocity is 1000 ~ 1200r/min, finally put into thermostat container, discharging after insulated and stirred 30 ~ 40min at 90 ~ 100 DEG C, after cooling, namely packaging obtains the fatty acid modified water-ground limestone of a kind of Semen Pericarpium Zanthoxyli.
CN201510951411.3A 2015-12-19 2015-12-19 Preparation method of Chinese prickly ash seed fatty acid modified heavy calcium carbonate Pending CN105419398A (en)

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Application publication date: 20160323