CN111875987A - Method for modifying wollastonite in factory - Google Patents

Method for modifying wollastonite in factory Download PDF

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Publication number
CN111875987A
CN111875987A CN202010763294.9A CN202010763294A CN111875987A CN 111875987 A CN111875987 A CN 111875987A CN 202010763294 A CN202010763294 A CN 202010763294A CN 111875987 A CN111875987 A CN 111875987A
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CN
China
Prior art keywords
wollastonite
stearic acid
factory
modifying
steps
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Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN202010763294.9A
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Chinese (zh)
Inventor
张艺梅
张晶
丁学宁
刘万龙
贾一鸣
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DALIAN HUANQIU MINERALS CO LTD
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DALIAN HUANQIU MINERALS CO LTD
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Publication date
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Priority to CN202010763294.9A priority Critical patent/CN111875987A/en
Publication of CN111875987A publication Critical patent/CN111875987A/en
Pending legal-status Critical Current

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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
    • C09C—TREATMENT 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
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/28—Compounds of silicon
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K7/00—Use of ingredients characterised by shape
    • C08K7/02—Fibres or whiskers
    • C08K7/04—Fibres or whiskers inorganic
    • C08K7/10—Silicon-containing compounds
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00—Use of pretreated ingredients
    • C08K9/04—Ingredients treated with organic substances
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT 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
    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/08—Treatment with low-molecular-weight non-polymer organic compounds
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING 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
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/60—Additives non-macromolecular
    • C09D7/61—Additives non-macromolecular inorganic
    • C09D7/62—Additives non-macromolecular inorganic modified by treatment with other compounds
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING 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
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/70—Additives characterised by shape, e.g. fibres, flakes or microspheres
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/21—Attrition-index or crushing strength of granulates

Abstract

The invention relates to a method for modifying wollastonite in a factory, belonging to the field of inorganic mineral fibers. The method comprises the following steps: adding 800 meshes of wollastonite into stearic acid ethanol aqueous solution, and carrying out modification reaction under sealing to obtain the modified wollastonite. The wollastonite and stearic acid used in the invention have low cost, the preparation method is simple, the requirements on production environment and equipment are not high, the wollastonite after surface modification treatment can improve the processing technique and remarkably improve the mechanical property of products when being added into a high polymer material, and the wollastonite has high economic value in industrial production.

Description

Method for modifying wollastonite in factory
Technical Field
The invention relates to a method for modifying wollastonite in a factory, belonging to the field of inorganic mineral fibers.
Background
Wollastonite of the formula CaSiO3It is a triclinic metasilicate mineral. Wollastonite is an inorganic acicular mineral, and has the characteristics of no toxicity, chemical corrosion resistance, good thermal stability and dimensional stability, glass and pearl luster, low water absorption rate and oil absorption value, excellent mechanical property and electrical property and certain reinforcing effect. The wollastonite product has long fiber length, easy separation, low iron content and high whiteness. The wollastonite product is mainly used as a reinforcing filler of a high polymer-based composite material and is widely applied to the industries of plastics, rubber, ceramics, coatings, building materials and the like.
Disclosure of Invention
After the wollastonite is crushed by mechanical force, stearic acid is added to modify the surface of the wollastonite, so that the dispersibility of the wollastonite in the wollastonite is further improved.
The invention provides a method for modifying wollastonite in a factory, which comprises the following steps: adding 800 meshes of wollastonite into stearic acid ethanol aqueous solution, and carrying out modification reaction under sealing to obtain the modified wollastonite.
The present invention preferably has the modification reaction conditions: the reaction is carried out for 30min at the temperature of 80-90 ℃, and the stirring speed of the reaction is 500-600 r/min.
The invention preferably selects the weight ratio of the wollastonite to the stearic acid as 1: 0.015-0.020.
The content of the stearic acid in the ethanol water solution is 2-5%.
The invention preferably has the volume ratio of the water to the ethanol of 1: 2.
the invention preferably adopts the following dissolving method of the stearic acid in the ethanol water solution: stirring at 500r/min for 30min at the temperature of 50-60 ℃.
The invention preferably selects the modified wollastonite obtained by cooling to room temperature after the modification reaction, separating the precipitate, washing, drying, grinding and screening.
The invention has the beneficial effects that:
the wollastonite and stearic acid used in the invention have low cost, the preparation method is simple, the requirements on production environment and equipment are not high, the wollastonite after surface modification treatment can improve the processing technique and remarkably improve the mechanical property of products when being added into a high polymer material, and the wollastonite has high economic value in industrial production.
Drawings
In the figure 2 of the attached drawings of the invention,
FIG. 1 is an infrared spectrum of modified wollastonite obtained in example 1;
FIG. 2 is an infrared spectrum of the modified wollastonite obtained in example 2.
Detailed Description
The following non-limiting examples are presented to enable those of ordinary skill in the art to more fully understand the present invention and are not intended to limit the invention in any way.
Example 1
A method for factory modifying wollastonite, comprising the steps of:
adding stearic acid into an ethanol water solution, heating to 60 ℃, stirring for 30min at 500r/min to dissolve the stearic acid, cooling to room temperature after dissolution, wherein the content of the stearic acid in the ethanol water solution is 2%, and the volume ratio of water to ethanol is 1: 2;
adding 800 meshes of wollastonite into the product obtained in the step I, reacting at 90 ℃ for 30min under sealing, stirring at the speed of 500r/min, cooling to room temperature after reaction, separating and precipitating, washing and precipitating for 2 times by using the ethanol aqueous solution, drying at 80 ℃, grinding and screening to obtain modified wollastonite, wherein the weight ratio of the wollastonite to stearic acid is 1: 0.020, the separated liquid can be reused.
As can be seen from FIG. 1, 1100--1The absorption bands of the asymmetric stretching vibration of Si-O-Si and the stretching vibration of O-Si-O are at 800--1The absorption peak is the symmetrical telescopic vibration absorption band of Si-O-Si of silicon-oxygen tetrahedron in the wollastonite structure; the wave number of the modified wollastonite is 2700-2849cm-1A stearic acid characteristic absorption peak appears at 1733cm-1Is widened and goes to low waveA small amount of displacement occurred in several directions, indicating that stearic acid had adhered to the wollastonite surface.
Example 2
A method for factory modifying wollastonite, comprising the steps of:
adding stearic acid into an ethanol water solution, heating to 60 ℃, stirring for 30min at 500r/min, dissolving stearic acid, and cooling to room temperature after dissolving, wherein the content of stearic acid in the ethanol water solution is 1%, 2%, 2.5% and 3%, the volume ratio of water to ethanol is 1: 2;
adding 800 meshes of wollastonite into the product obtained in the step I, reacting at 90 ℃ for 30min under sealing, stirring at the reaction speed of 500r/min, cooling to room temperature after reaction, separating and precipitating, washing and precipitating for 2 times by using the ethanol aqueous solution, drying at 80 ℃, grinding and screening to obtain modified wollastonite, wherein the infrared spectroscopic analysis of the modified wollastonite is as follows, and the weight ratio of the wollastonite to stearic acid is 1: 0.010, 1: 0.020, 1: 0.025, 1: 0.030, the separated liquid can be reused
As shown in FIG. 2, the stearic acid modified wollastonite with different mass fractions is 1500-1600cm-1New absorption peaks appear; the absorption peak of the calcium stearate is analyzed to be an antisymmetric stretching vibration absorption peak of C ═ O bonds in the calcium stearate, and the peak value is enhanced along with the increase of the mass fraction of the stearic acid.
Example 3
Experiment of activation Rate
Adding 100mL of water into a separating funnel, weighing 10g of modified wollastonite, adding the modified wollastonite into the separating funnel, adding 100mL of water, oscillating for 1min at the speed of 120 times/min, standing for 24h, layering, then leaking out the deposit on the lower layer, drying at 110 ℃ to constant weight Sg, and obtaining the activation rate result shown in Table 1 below.
TABLE 1
Stearic acid mass fraction (%) 1.0 1.5 2.0 2.5 3.0
Activation ratio (%) 91.86 93.78 95.69 95.21 94.76
Remarking: the activation index is: h ═ 10-S)/10
As can be seen from Table 1, the activation rate increases with the increase of the stearic acid mass fraction; when the mass fraction of stearic acid is 2%, the activation rate is 95.69%, and the maximum value is reached; the activation rate tends to decrease as the mass fraction of stearic acid continues to increase.
Example 4
Tensile Strength test
The tensile strength of the modified wollastonite/polypropylene is tested by adopting a two-roll open mill for mixing and a flat vulcanizing machine for vulcanization molding, the physical and mechanical properties of a polypropylene test piece are tested according to GB/T1040-
TABLE 2
Stearic acid mass fraction (%) 0 1.0 1.5 2.0 2.5 3.0
Tensile Strength (MPa) 22.56 24.63 26.75 27.28 24.29 23.51
As can be seen from Table 2, the tensile strength increases with the increase in the mass fraction of stearic acid; when the mass fraction of stearic acid is 2%, the tensile strength is 27.28MPa, and the maximum value is reached; the tensile strength tends to decrease as the mass fraction of stearic acid continues to increase.

Claims (7)

1. A method for modifying wollastonite in factory is characterized by comprising the following steps: the method comprises the following steps:
adding 800 meshes of wollastonite into stearic acid ethanol aqueous solution, and carrying out modification reaction under sealing to obtain the modified wollastonite.
2. The method for factory modifying wollastonite of claim 1, comprising the steps of: the conditions of the modification reaction are as follows: the reaction is carried out for 30min at the temperature of 80-90 ℃, and the stirring speed of the reaction is 500-600 r/min.
3. The method for factory modifying wollastonite of claim 2, wherein: the weight ratio of the wollastonite to the stearic acid is 1: 0.015-0.020.
4. The method for factory modifying wollastonite of claim 3, wherein the method comprises the steps of: the content of stearic acid in the ethanol water solution is 2-5%.
5. The method for factory modifying wollastonite of claim 4, wherein the method comprises the steps of: the volume ratio of the water to the ethanol is 1: 2.
6. the method for factory modifying wollastonite of claim 5, wherein the method comprises the steps of: the method for dissolving stearic acid in the ethanol water solution comprises the following steps: stirring at 500r/min for 30min at the temperature of 50-60 ℃.
7. The method for factory modifying wollastonite of claim 6, comprising the steps of: and cooling to room temperature after the modification reaction, separating and precipitating, washing, drying, grinding and screening to obtain the modified wollastonite.
CN202010763294.9A 2020-07-31 2020-07-31 Method for modifying wollastonite in factory Pending CN111875987A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114410130A (en) * 2021-11-23 2022-04-29 江西广源化工有限责任公司 Modified wollastonite and preparation method and application thereof
CN115521696A (en) * 2022-09-30 2022-12-27 李承杰 Wear-resistant polyurethane coating and preparation method thereof

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4420341A (en) * 1982-04-05 1983-12-13 Ferrigno Thomas H Stabilized surface modified fillers
CN101139469A (en) * 2007-07-30 2008-03-12 中国地质大学（武汉） Modification method for protecting crystal form of grammite
CN102532951A (en) * 2011-10-28 2012-07-04 华东理工大学 Method for toughening epoxy resin by adopting modified wollastonite
CN103435974A (en) * 2013-09-09 2013-12-11 郴州四方立投资有限公司 Preparation method of modified wollastonite used for toughening epoxy resin
CN106381124A (en) * 2016-10-13 2017-02-08 常州创索新材料科技有限公司 Preparation method of high-stability waterproof roll

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4420341A (en) * 1982-04-05 1983-12-13 Ferrigno Thomas H Stabilized surface modified fillers
CN101139469A (en) * 2007-07-30 2008-03-12 中国地质大学（武汉） Modification method for protecting crystal form of grammite
CN102532951A (en) * 2011-10-28 2012-07-04 华东理工大学 Method for toughening epoxy resin by adopting modified wollastonite
CN103435974A (en) * 2013-09-09 2013-12-11 郴州四方立投资有限公司 Preparation method of modified wollastonite used for toughening epoxy resin
CN106381124A (en) * 2016-10-13 2017-02-08 常州创索新材料科技有限公司 Preparation method of high-stability waterproof roll

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114410130A (en) * 2021-11-23 2022-04-29 江西广源化工有限责任公司 Modified wollastonite and preparation method and application thereof
CN115521696A (en) * 2022-09-30 2022-12-27 李承杰 Wear-resistant polyurethane coating and preparation method thereof

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