CN105504891A - Preparation method of rare earth modifier - Google Patents

Preparation method of rare earth modifier Download PDF

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Publication number
CN105504891A
CN105504891A CN201510880351.0A CN201510880351A CN105504891A CN 105504891 A CN105504891 A CN 105504891A CN 201510880351 A CN201510880351 A CN 201510880351A CN 105504891 A CN105504891 A CN 105504891A
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China
Prior art keywords
rare
nitrate
rare earth
earth modifier
earth
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Pending
Application number
CN201510880351.0A
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Chinese (zh)
Inventor
李军伟
商冬洁
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TIANJIN RUCHUANG NEW MATERIALS TECHNOLOGY Co Ltd
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TIANJIN RUCHUANG NEW MATERIALS TECHNOLOGY Co Ltd
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Priority to CN201510880351.0A priority Critical patent/CN105504891A/en
Publication of CN105504891A publication Critical patent/CN105504891A/en
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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
    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/006—Combinations of treatments provided for in groups C09C3/04 - C09C3/12
    • 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
    • C09C1/02—Compounds of alkaline earth metals or magnesium
    • C09C1/021—Calcium carbonates
    • 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
    • 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
    • C09C3/12—Treatment with organosilicon compounds

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)

Abstract

The invention provides a preparation method of a rare earth modifier. Firstly, rare earth nitrate is dissolved in ethanol, then salicylic acid is added, the molar ratio of the rare earth nitrate to the salicylic acid is controlled to be 1:4.1, the temperature is increased to 80 DEG C, a sodium hydroxide-ethanol solution is slowly dropwise added, the molar ratio of sodium hydroxide to the salicylic acid is controlled to be 3.1:1, the mixture reacts for 3 h after addition, then the pH value of the system is adjusted to be 4-6, the system reacts at the temperature of 80 DEG C for 1 h and is filtered after being left to stand for 20 min, a white precipitate is obtained, an intermediate is obtained through water washing, alcohol washing and drying, finally, the intermediate is added to deionized water, hydrochloric acid is dropwise added to adjust the pH value until the intermediate is completely dissolved, the intermediate is slowly dropwise added to tetraethyl orthosilicate with violent stirring, the mas ratio of the intermediate to the tetraethyl orthosilicate is controlled to be 1:20, the mixture reacts at the temperature of 30 DEG C for 8h and is left to stand for 36 h, and the rare earth modifier is prepared. The rare earth modifier has a good activation effect, has plasticizing and lubricating functions and the like and can be applied to the field of inorganic powder surface modification.

Description

A kind of preparation method of rare-earth modifier
Technical field
The invention belongs to surface-modifying agent preparation field, relate to a kind of preparation method of rare-earth modifier.
Background technology
The gordian technique that restriction inorganic powder is applied in macromolecular material matrix how to improve both interface binding powers, coupling agent can be adopted to carry out surface modification to inorganic powder, in plastics are compounding, the face performance of organic plastics and inorganic powder can be improved, improve the interface binding power between inorganic powder and organic matrix, thus promote the overall performance of matrix material.The kind of conventional coupling agent comprises silicane, titanate ester, aluminate etc., various coupling agent has different modified effects, along with the development of matrix material, demand for Multifunction coupling agent is more urgent, there is Hot Contents that synergistic compound coupling agent has become coupling agent research at present, meet the development trend of coupling agent, therefore develop applied widely, that potion multipotency, activation effect better, cost is cheaper novel coupling agent and there is good researching value.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, provide a kind of preparation method of rare-earth modifier, the rare-earth modifier activation effect of preparation is good, and has the function such as plasticising, lubrication, can be applicable to Surface Modification of Inorganic Powder field, and modified effect is good.
For realizing above object, the technical solution used in the present invention is:
A preparation method for rare-earth modifier, comprises the following steps:
(1) take rare earth nitrate to be dissolved in dehydrated alcohol, then add Whitfield's ointment, control rare earth nitrate and salicylic mol ratio are 1:4.1, be warming up to 80 DEG C, slowly drip sodium hydroxide-ethanolic soln, control sodium hydroxide and salicylic mol ratio are 3.1:1, dropwise rear reaction 3h, the pH value of regulation system is react 1h at 4 ~ 6,80 DEG C, filters after leaving standstill 20min, obtain white depositions, white depositions is washed repeatedly, alcohol wash, vacuum drying, obtains intermediate;
(2) intermediate is added in deionized water, drip salt acid for adjusting pH value until intermediate dissolves completely, then it is slowly added dropwise in tetraethoxy, violent stirring, the mass ratio of control and intermediate and tetraethoxy is 1:20, at 30 DEG C, react 8h, leave standstill and to obtain outward appearance after 36h and to be creamy white transparent rare-earth modifier.
Described rare earth nitrate is the mixture of one or more of lanthanum nitrate, cerous nitrate, neodymium nitrate.
Described rare-earth modifier is applied to the surface modification of inorganic powder.
Beneficial effect of the present invention:
The invention provides a kind of preparation method of rare-earth modifier, with Whitfield's ointment and rare earth nitrate for raw material, first salicylate Lanthanide complex, sol-gel technique is adopted to be re-dubbed salicylic acid type rare-earth modifier again, present method technique is simple, and the rare-earth modifier activation effect of preparation is good, and has the function such as plasticising, lubrication, be applicable to carry out surface modification to inorganic powder, modified effect is good.
Accompanying drawing explanation
Fig. 1 is the infrared spectrogram of the embodiment of the present invention 1 rare-earth modifier;
Fig. 2 is the DSC figure of the embodiment of the present invention 1 rare-earth modifier;
Fig. 3 is the TG figure of the embodiment of the present invention 1 rare-earth modifier.
Embodiment
In order to make technical problem solved by the invention, technical scheme and beneficial effect clearly understand, below in conjunction with embodiment, the present invention is further illustrated.Should be appreciated that embodiment described herein only for explaining the present invention, being not intended to limit the present invention.
embodiment 1
A preparation method for rare-earth modifier, comprises the following steps:
(1) take lanthanum nitrate to be dissolved in dehydrated alcohol, then add Whitfield's ointment, control lanthanum nitrate and salicylic mol ratio are 1:4.1, be warming up to 80 DEG C, slowly drip sodium hydroxide-ethanolic soln, control sodium hydroxide and salicylic mol ratio are 3.1:1, dropwise rear reaction 3h, the pH value of regulation system is react 1h at 5.5,80 DEG C, filters after leaving standstill 20min, obtain white depositions, white depositions is washed repeatedly, alcohol wash, vacuum drying, obtains intermediate;
(2) intermediate is added in deionized water, drip salt acid for adjusting pH value until intermediate dissolves completely, then it is slowly added dropwise in tetraethoxy, violent stirring, the mass ratio of control and intermediate and tetraethoxy is 1:20, at 30 DEG C, react 8h, leave standstill and to obtain outward appearance after 36h and to be creamy white transparent rare-earth modifier.
Characterize rare-earth modifier prepared by embodiment 1, what the infrared spectrogram of Fig. 1 showed rare-earth modifier consists of Lanthanum salicylate, and it is better that the TG of the DSC figure and Fig. 3 of Fig. 2 schemes all to show this rare-earth modifier thermal stability.
Simultaneously in order to characterize embodiment 1 rare-earth modifier to the surface modification effect of inorganic powder, this rare-earth modifier is adopted to carry out surface modification to calcium carbonate, test its degree of activation, and by non-modified and modified calcium carbonate respectively filled polypropylene prepare matrix material, the mechanical property of test compound material, to characterize the surface modification effect of rare-earth modifier to calcium carbonate.Step is as follows:
(1) rare-earth modifier modified calcium carbonate: 10g rare-earth modifier is added in 1Kg calcium carbonate, in homogenizer at 80 DEG C high-speed stirring 15min, obtain modified calcium carbonate;
(2) degree of activation of modified calcium carbonate: disperseed in deionized water by modified calcium carbonate, stirs 25min at 60 DEG C, and take out the floating calcium carbonate in upper strata after leaving standstill, oven dry is weighed, and is degree of activation with the ratio of calcium carbonate total amount.Test result shows: the degree of activation of modified calcium carbonate reaches 98.1%, visible, and the activation effect of the present embodiment rare-earth modifier to calcium carbonate is better;
(3) the preparation and property test of polypropylene composite material: the calcium carbonate 2Kg and the modified calcium carbonate 2Kg that weigh non-modified add in 8KgPP respectively, forcing machine is adopted to melt extrude granulation after pre-mixing, obtain unmodified calcium carbonate/polypropylene composite material and modified calcium carbonate/polypropylene composite material, injection moulding machine is adopted to be injection molded into test bars respectively again, tensile property test is carried out to test bars, test result is as follows: polypropylene, the tensile strength of unmodified calcium carbonate/polypropylene composite material and modified calcium carbonate/polypropylene composite material is respectively 2.25MPa, 1.72MPa and 1.98MPa, visible, calcium carbonate is after rare-earth modifier surface modification, provide the mechanical property of matrix material.
embodiment 2
A preparation method for rare-earth modifier, comprises the following steps:
(1) take cerous nitrate to be dissolved in dehydrated alcohol, then add Whitfield's ointment, control cerous nitrate and salicylic mol ratio are 1:4.1, be warming up to 80 DEG C, slowly drip sodium hydroxide-ethanolic soln, control sodium hydroxide and salicylic mol ratio are 3.1:1, dropwise rear reaction 3h, the pH value of regulation system is react 1h at 5,80 DEG C, filters after leaving standstill 20min, obtain white depositions, white depositions is washed repeatedly, alcohol wash, vacuum drying, obtains intermediate;
(2) intermediate is added in deionized water, drip salt acid for adjusting pH value until intermediate dissolves completely, then it is slowly added dropwise in tetraethoxy, violent stirring, the mass ratio of control and intermediate and tetraethoxy is 1:20, at 30 DEG C, react 8h, leave standstill and to obtain outward appearance after 36h and to be creamy white transparent rare-earth modifier.
embodiment 3
A preparation method for rare-earth modifier, comprises the following steps:
(1) take neodymium nitrate to be dissolved in dehydrated alcohol, then add Whitfield's ointment, control neodymium nitrate and salicylic mol ratio are 1:4.1, be warming up to 80 DEG C, slowly drip sodium hydroxide-ethanolic soln, control sodium hydroxide and salicylic mol ratio are 3.1:1, dropwise rear reaction 3h, the pH value of regulation system is react 1h at 4,80 DEG C, filters after leaving standstill 20min, obtain white depositions, white depositions is washed repeatedly, alcohol wash, vacuum drying, obtains intermediate;
(2) intermediate is added in deionized water, drip salt acid for adjusting pH value until intermediate dissolves completely, then it is slowly added dropwise in tetraethoxy, violent stirring, the mass ratio of control and intermediate and tetraethoxy is 1:20, at 30 DEG C, react 8h, leave standstill and to obtain outward appearance after 36h and to be creamy white transparent rare-earth modifier.
Above-described embodiment is only one of preferred embodiment of the present invention, not limits the scope of the invention with this, therefore: all equivalence changes done according to structure of the present invention, shape, principle, all should be covered by within protection scope of the present invention.

Claims (3)

1. a preparation method for rare-earth modifier, is characterized in that: comprise the following steps:
(1) take rare earth nitrate to be dissolved in dehydrated alcohol, then add Whitfield's ointment, control rare earth nitrate and salicylic mol ratio are 1:4.1, be warming up to 80 DEG C, slowly drip sodium hydroxide-ethanolic soln, control sodium hydroxide and salicylic mol ratio are 3.1:1, dropwise rear reaction 3h, the pH value of regulation system is react 1h at 4 ~ 6,80 DEG C, filters after leaving standstill 20min, obtain white depositions, white depositions is washed repeatedly, alcohol wash, vacuum drying, obtains intermediate;
(2) intermediate is added in deionized water, drip salt acid for adjusting pH value until intermediate dissolves completely, then it is slowly added dropwise in tetraethoxy, violent stirring, the mass ratio of control and intermediate and tetraethoxy is 1:20, at 30 DEG C, react 8h, leave standstill and to obtain outward appearance after 36h and to be creamy white transparent rare-earth modifier.
2. the preparation method of rare-earth modifier according to claim 1, is characterized in that: described rare earth nitrate is the mixture of one or more of lanthanum nitrate, cerous nitrate, neodymium nitrate.
3. the preparation method of rare-earth modifier according to claim 1, is characterized in that: described rare-earth modifier is applied to the surface modification of inorganic powder.
CN201510880351.0A 2015-12-06 2015-12-06 Preparation method of rare earth modifier Pending CN105504891A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106478987A (en) * 2016-10-24 2017-03-08 天津城建大学 A kind of waste stone dust surface modifying method based on dry grinding
CN107541166A (en) * 2016-06-24 2018-01-05 李澄 Rare earth oxyhalide silicate nanometer removes the preparation method of aldehyde modifying agent

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102503549A (en) * 2011-11-02 2012-06-20 上海大学 Preparation method for polycrystalline thin film made of lutecium silicate doped with rare earth ions
CN102500291A (en) * 2011-09-30 2012-06-20 深圳市易瑞生物技术有限公司 Preparation method and application of magnetic fluorescent nanoparticle with shell-core structure
CN102504808A (en) * 2011-10-19 2012-06-20 厦门大学 Preparation method of rare-earth fluorescent silica nano particle
CN102876322A (en) * 2012-10-24 2013-01-16 上海理工大学 Rare-earth polyurethane high-polymer composite luminescent material and preparation method thereof
CN104479415A (en) * 2014-12-26 2015-04-01 天津滨浦生产力促进有限公司 Calcium carbonate surface modifier

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102500291A (en) * 2011-09-30 2012-06-20 深圳市易瑞生物技术有限公司 Preparation method and application of magnetic fluorescent nanoparticle with shell-core structure
CN102504808A (en) * 2011-10-19 2012-06-20 厦门大学 Preparation method of rare-earth fluorescent silica nano particle
CN102503549A (en) * 2011-11-02 2012-06-20 上海大学 Preparation method for polycrystalline thin film made of lutecium silicate doped with rare earth ions
CN102876322A (en) * 2012-10-24 2013-01-16 上海理工大学 Rare-earth polyurethane high-polymer composite luminescent material and preparation method thereof
CN104479415A (en) * 2014-12-26 2015-04-01 天津滨浦生产力促进有限公司 Calcium carbonate surface modifier

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
张秀英，张有娟，雷雪峰: "水杨酸稀土配合物的研究进展", 《稀土》 *
朱文婷: "稀土杂化发光材料的制备及性能研究", 《中国优秀硕士学位论文全文数据库》 *
赵贞: "新型稀土偶联剂的合成及应用研究", 《中国优秀硕士学位论文全文数据库》 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107541166A (en) * 2016-06-24 2018-01-05 李澄 Rare earth oxyhalide silicate nanometer removes the preparation method of aldehyde modifying agent
CN106478987A (en) * 2016-10-24 2017-03-08 天津城建大学 A kind of waste stone dust surface modifying method based on dry grinding
CN106478987B (en) * 2016-10-24 2018-07-03 天津城建大学 A kind of waste stone dust surface modifying method based on dry grinding

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Application publication date: 20160420