CN106398320A - Preparation method and application of high-modulus modified talcum powder - Google Patents

Preparation method and application of high-modulus modified talcum powder Download PDF

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Publication number
CN106398320A
CN106398320A CN201610783253.XA CN201610783253A CN106398320A CN 106398320 A CN106398320 A CN 106398320A CN 201610783253 A CN201610783253 A CN 201610783253A CN 106398320 A CN106398320 A CN 106398320A
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China
Prior art keywords
talcum powder
silane coupler
modulus
preparation
powder
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Pending
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CN201610783253.XA
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Chinese (zh)
Inventor
施伟章
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Quanzhou Xu Feng Powder Raw Materials Co Ltd
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Quanzhou Xu Feng Powder Raw Materials Co Ltd
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Priority to CN201610783253.XA priority Critical patent/CN106398320A/en
Publication of CN106398320A publication Critical patent/CN106398320A/en
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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
    • C09C1/28Compounds of silicon
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/34Silicon-containing compounds
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00Use of pretreated ingredients
    • C08K9/04Ingredients treated with organic substances
    • C08K9/06Ingredients treated with organic substances with silicon-containing compounds
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00Use of pretreated ingredients
    • C08K9/10Encapsulated ingredients
    • 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
    • C09C3/12Treatment with organosilicon compounds
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/002Physical properties
    • C08K2201/003Additives being defined by their diameter

Abstract

The invention discloses a preparation method for high-modulus modified talcum powder. The preparation method comprises the following steps: subjecting talcum powder to stirring at a low rotating speed of no more than 600 r/min in a high-speed mixer equipped with a guiding grove; adding a silane coupling agent through cold treatment drop by drop in three steps, wherein the addition amounts of the silane coupling agent successively decrease in the three steps, and allowing the silane coupling agent to adequately react with talcum powder; and successively carrying out heating to 90 to 120 DEG C, high-speed stirring at a rotating speed of no less than 1400 r/min and adequate reaction for 25 to 35 min so as to obtain the high-modulus modified talcum powder. The high-modulus modified talcum powder prepared in the invention has good interfacial compatibility with a PP matrix; and when applied to talcum powder-filled PP products as a non-mineral filler, the high-modulus modified talcum powder enables the PP products to have high modulus and high flow ratio.

Description

A kind of preparation method and application of high-modulus modified talc powder
Technical field
The present invention relates to powder technology field and in particular to be a kind of preparation method of high-modulus modified talc powder and should With.
Background technology
Polypropylene (PP) is wide variety of a kind of general-purpose plastics both at home and abroad, has widely applied auto parts and components, household electrical appliances system The most macromolecular material of consumption in the industries such as product, particularly automobile, Automobile Part bumper, instrument board, wheel cover, door-plate, starts Many parts such as hood, air conditioner housing, console, horn hood are the product part that MODIFIED PP material produces two layers.In order to improve PP Mechanical property reduces cost simultaneously, often modification is filled with to PP polymer using the non-ore deposit filler such as talcum powder.MODIFIED PP To PP modified materials, the application on automobile has a very big impact the modulus height of material, is also to ensure that of product quality simultaneously Importance, the height of MODIFIED PP material mobility has very big impact to injection member aspect.
Talcum powder is a kind of cheap, resourceful inorganic filler, can improve the shaping of plastics after filled plastics Shrinkage.In order to improve mechanical property, improve the consistency problem of talcum powder and PP, modified producer is in processing MODIFIED PP In material, directly mixing can add silane coupler, lift product part intensity.But directly mix coupling agent, in extrusion process, Volatile byproducts are easily caused other problems and produce, the talcous water imbibition of reduction is not improved, and modifying agent is in liquid form Add and easily mix uneven, especially high-end super fine, easily disperse uneven, soft-agglomerated phenomenon easily occurs.
Content of the invention
It is an object of the invention to provide a kind of preparation method of high-modulus modified talc powder, the high-modulus preparing changes Property talcum powder and PP base-material there is good interface compatibility, this high-modulus modified talc powder is applied to as Non-mineral fillers In talc PP product, it is possible to increase MODIFIED PP product high-modulus, the performance of high flowing ratio.
In order to reach above-mentioned purpose, the solution of the present invention is:
A kind of preparation method of high-modulus modified talc powder, comprises the following steps:
(1) talcum powder is added in the homogenizer with guiding gutter, in the stirring at low speed of rotating speed≤600r/min Lower stirring;
(2) it is added in an amount of the silane coupler of the 0.8-1.5wt% of described amount of talc in described talcum powder, will Described silane coupler is added drop-wise in talcum powder according to principle of successively decreasing several times, and the interval time of each dropwise operation is 3- 5min;
(3) be warming up to 90-120 DEG C, in rotating speed be >=high-speed stirred of 1400r/min under stir, fully react 25- 35min, that is, prepare this high-modulus modified talc powder.
In step (1), the talcum powder that described talcum powder is 5~7um from average grain diameter.
In step (2), described silane coupler is silane coupler D-9.
In step (2), inequality is added drop-wise in talcum powder described silane coupler in three times, and the silane of dropping is even for the first time The consumption of connection agent is the 60% of described silane coupler total amount, and the consumption of the silane coupler of second dropping is that described silane is even The 25% of connection agent total amount, the consumption of the silane coupler of third time dropping is the 15% of described silane coupler total amount.
Application in talc PP product for the above-mentioned high-modulus modified talc powder.
A kind of preparation method of present invention high-modulus modified talc powder, has the advantage that:
(1) talcum powder is added in the homogenizer have guiding gutter and is prepared, powder can be reduced and stick wall phenomenon, The electric heater unit quick heating of homogenizer, makes reaction more abundant;
(2) silane coupler is added drop-wise to several times the effect in talcum powder according to principle of successively decreasing:Make powder surface complete Cladding, improves the activation rate of powder, improves performance in PP product for the talcum powder powder, in addition, silane coupler is as talcum " bridge " of powder and PP base-material, can improve the interface compatibility between modified talc powder and PP base-material, have concurrently simultaneously high-modulus, The performance of high fluidity;
(3) after silane coupler is sufficiently mixed with talcum powder, the rotating speed of homogenizer is adjusted at a high speed, fully react 25-35min, the reaction time is too short not to reach talcous modified effect, and activation rate is low, and the reaction time is long will to bring power consumption to increase Plus, production efficiency reduces, powder sticks the phenomenon that increases of wall.
The high-modulus modified talc powder being prepared by a kind of preparation method of present invention high-modulus modified talc powder and PP Base-material has good interface compatibility, and this high-modulus modified talc powder is applied to talc PP as Non-mineral fillers In product, it is possible to increase MODIFIED PP product high-modulus, the performance of high flowing ratio.
Further, in step (1), the talcum powder that described talcum powder is 5~7um from average grain diameter, talcum powder is filled out Fill during PP base-material from sexual valence when processing characteristics optimum, be less prone to bridge formation and emit powder phenomenon.
Further, in step (2), inequality is added drop-wise in talcum powder described silane coupler in three times, drips for the first time The consumption of silane coupler be the 60% of described silane coupler total amount, the consumption of the silane coupler of second dropping is institute State the 25% of silane coupler total amount, the consumption of the silane coupler of third time dropping is described silane coupler total amount 15% so that silane coupler is fully reacted with talcum powder.
Specific embodiment
In order to technical scheme is explained further, the present invention is explained in detail below by specific embodiment State.
Embodiment one
1st, prepare
A kind of preparation method of high-modulus modified talc powder, comprises the following steps:
(1) talcum powder is added in the homogenizer with guiding gutter, in the stirring at low speed of rotating speed≤600r/min Lower stirring;
(2) it is added in an amount of the silane coupler of the 1.5wt% of amount of talc in talcum powder, silane coupler is divided It is added drop-wise in talcum powder for three times, drip the 60% of silane coupler total amount for the first time, second dropping silane coupler total amount 25%, third time drips the 15% of silane coupler total amount, and the interval time of each dropwise operation is 5min, fully mixes;
(3) be warming up to 90-120 DEG C, in rotating speed be >=high-speed stirred of 1400r/min under stir, fully react 30min, Prepare this high-modulus modified talc powder.
In step (1), the talcum powder that talcum powder is 5~7um from average grain diameter.
In step (2), silane coupler is silane coupler D-9, creates the limited public affairs of Degussa Specialty Chemical (Shanghai) by winning Department's supply.
2nd, performance test
By unmodified talc, in PP resin, (based on homopolymerization PP Y2600T resin is set supplemented by copolymerization PP K8003 Fat), the sample 1 of preparation 20% talc PP, by unmodified talc when the PP resin directly interpolation silane coupled Agent, the sample 2 of preparation 20% talc PP, PP will be filled in by the modified talc powder that the preparation method invented prepares Resin, preparation 20% modified talc powder fills the sample 3 of PP, tests each sample performance, and as shown in table 1, result shows result: With the modified talc powder filling PP sample of the method preparation, the performance comparison with other two kinds of samples, bending modulus amplification 32.1%, melt index amplification 47%, thus improve the performance of product, meet the demand to high-quality finished product for the producer.Pass through Synthetic performance evaluation, has the characteristics that high-modulus, high fluidity by modified talc powder prepared by this preparation method.
The properties test data of each sample of table 1
Embodiment two
1st, prepare
A kind of preparation method of high-modulus modified talc powder, comprises the following steps:
(1) talcum powder is added in the homogenizer with guiding gutter, in the stirring at low speed of rotating speed≤600r/min Lower stirring;
(2) it is added in an amount of the silane coupler of the 0.8wt% of amount of talc in talcum powder, less than 80 DEG C At a temperature of silane coupler is added drop-wise in talcum powder in three times, drip for the first time the 60% of silane coupler total amount, second The 25% of dropping silane coupler total amount, third time drips the 15% of silane coupler total amount, during the interval of each dropwise operation Between be 3min, fully mix;
(3) be warming up to 90-120 DEG C, in rotating speed be >=high-speed stirred of 1400r/min under stir, fully react 25min, Prepare this high-modulus modified talc powder.
In step (1), talcum powder selects the talcum powder that average grain diameter is 7um, in order to contrast, in the present embodiment, talcum powder Also it is modified for the talcum powder of 1um and 4um from average grain diameter.
In step (2), silane coupler is silane coupler D-9, create the limited public affairs of Degussa Specialty Chemical (Shanghai) by winning Department's supply.
2nd, performance test
The modified talc powder that the average grain diameter of talcum powder (import) is 1um is filled in PP resin (with homopolymerization PP Y2600T Based on resin, resin supplemented by copolymerization PP K8003), the sample 4 of preparation 20% talc PP, by talcum powder (domestic high-end) Average grain diameter be that the modified talc powder of 4um is filled in PP resin, the sample 5 of preparation 20% talc PP, by talcum powder Average grain diameter be that the modified talc powder of 7um is filled in PP resin, preparation 20% modified talc powder fills the sample 6 of PP, test Each sample performance, as shown in table 2, result shows result:Compared with sample 4 and sample 5, the bending strength of sample 6, melting refer to Number all increases, and modified talc powder filling PP has advantage in performance, from the modified talc powder for 7um for the average grain diameter is Filler in MODIFIED PP, may also operate as the effect of melt flows accelerator, modified talcum powder, not only can meet factory The requirements at the higher level to product for the family, also reduce the product cost of high-quality finished product.
The properties test data of each sample of table 2
The product form of above-described embodiment the non-limiting present invention and style, the ordinary skill people of any art Suitable change or modification that member is done to it, all should be regarded as the patent category without departing from the present invention.

Claims (5)

1. a kind of preparation method of high-modulus modified talc powder it is characterised in that:Comprise the following steps:
(1) talcum powder is added in the homogenizer with guiding gutter, stirs under the stirring at low speed of rotating speed≤600r/min Mix;
(2) it is added in an amount of the silane coupler of the 0.8-1.5wt% of described amount of talc in described talcum powder, do not surpassing Cross and at a temperature of 80 DEG C, described silane coupler is added drop-wise in talcum powder according to principle of successively decreasing several times, each dropwise operation Interval time is 3-5min;
(3) be warming up to 90-120 DEG C, in rotating speed be >=high-speed stirred of 1400r/min under stir, fully react 25-35min, that is, Prepare this high-modulus modified talc powder.
2. a kind of high-modulus modified talc powder according to claim 1 preparation method it is characterised in that:In step (1), The talcum powder that described talcum powder is 5~7um from average grain diameter.
3. a kind of high-modulus modified talc powder according to claim 1 preparation method it is characterised in that:In step (2), Described silane coupler is silane coupler D-9.
4. a kind of high-modulus modified talc powder according to claim 1 preparation method it is characterised in that:In step (2), Inequality is added drop-wise in talcum powder described silane coupler in three times, and the consumption of the silane coupler of dropping is described silicon for the first time The 60% of alkane coupling agent total amount, the consumption of the silane coupler of second dropping is the 25% of described silane coupler total amount, the The consumption of the silane coupler of three droppings is the 15% of described silane coupler total amount.
5. the described high-modulus that a kind of preparation method of high-modulus modified talc powder according to claim 1 prepares changes Property application in talc PP product for the talcum powder.
CN201610783253.XA 2016-08-31 2016-08-31 Preparation method and application of high-modulus modified talcum powder Pending CN106398320A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107793794A (en) * 2017-10-12 2018-03-13 桂林浩新科技服务有限公司 A kind of method for preparing monolithic talcum powder
CN107858020A (en) * 2017-10-12 2018-03-30 桂林浩新科技服务有限公司 A kind of method for preparing monolithic talcum powder
CN108359137A (en) * 2017-12-29 2018-08-03 柳州市海达新型材料科技有限公司 A kind of preparation method of low bulk modified talc powder
CN108929572A (en) * 2018-08-06 2018-12-04 宁波普莱斯帝金属制品有限公司 A kind of preparation method being alkylated superfine talcum powder
CN109111634A (en) * 2018-08-06 2019-01-01 宁波普莱斯帝金属制品有限公司 A kind of preparation method being alkylated superfine talcum powder modified poly ethylene

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CN102127261A (en) * 2011-01-07 2011-07-20 海城精华矿产有限公司 Special scratch-resistant talcum powder for polypropylene and preparation method thereof
CN103642124A (en) * 2013-11-21 2014-03-19 桂林福冈新材料有限公司 Preparation method of polypropylene car bumper

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107793794A (en) * 2017-10-12 2018-03-13 桂林浩新科技服务有限公司 A kind of method for preparing monolithic talcum powder
CN107858020A (en) * 2017-10-12 2018-03-30 桂林浩新科技服务有限公司 A kind of method for preparing monolithic talcum powder
CN108359137A (en) * 2017-12-29 2018-08-03 柳州市海达新型材料科技有限公司 A kind of preparation method of low bulk modified talc powder
CN108929572A (en) * 2018-08-06 2018-12-04 宁波普莱斯帝金属制品有限公司 A kind of preparation method being alkylated superfine talcum powder
CN109111634A (en) * 2018-08-06 2019-01-01 宁波普莱斯帝金属制品有限公司 A kind of preparation method being alkylated superfine talcum powder modified poly ethylene
CN108929572B (en) * 2018-08-06 2020-06-16 宁波普莱斯帝金属制品有限公司 Preparation method of alkylated superfine talcum powder

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Inventor after: Liu Kai

Inventor before: Shi Weizhang

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Application publication date: 20170215