CN102352132A - Method for preparing hydrophobic barium carbonate - Google Patents

Method for preparing hydrophobic barium carbonate Download PDF

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Publication number
CN102352132A
CN102352132A CN2011102414737A CN201110241473A CN102352132A CN 102352132 A CN102352132 A CN 102352132A CN 2011102414737 A CN2011102414737 A CN 2011102414737A CN 201110241473 A CN201110241473 A CN 201110241473A CN 102352132 A CN102352132 A CN 102352132A
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Prior art keywords
barium carbonate
hydrophobicity
properties
barium
correcting agent
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CN2011102414737A
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Chinese (zh)
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霍冀川
刘铭
刘树信
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Southwest University of Science and Technology
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Southwest University of Science and Technology
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Priority to CN2011102414737A priority Critical patent/CN102352132A/en
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Abstract

The invention discloses a method for preparing hydrophobic barium carbonate, which is characterized by comprising the following steps of: taking barium carbonate and a modifying agent accounting for 0.1-20% of barium carbonate by weight, mixing the barium carbonate with the modifying agent, and agitating the mixture at the temperature of 50-170 DEG C to react for 5-120 min to obtain the hydrophobic barium carbonate, wherein the modifying agent is a stearic acid or aluminate ester coupling agent. By using the method provided by the invention, the raw materials are easy to acquire, the production process is easy to implement, and the obtained modified barium carbonate can be used as a filling material of plastics, rubber, coatings and the like and has broad application prospect.

Description

A kind of preparation method of hydrophobicity barium carbonate
Technical field
The invention belongs to the preparation method of surface modification carbonic acid barium, relate to a kind of preparation method of hydrophobicity barium carbonate.The hydrophobicity barium carbonate particularly suitable that adopts the present invention to prepare is made the stopping composition of plastics, rubber, coating etc.
Background technology
In the prior art, barium carbonate is widely used in industries such as plastics, rubber and coating as filling-modified material, both can improve the dimensional stability etc. of rigidity, hardness, wear resistance, thermotolerance and the goods of matrix material, can reduce the cost of goods again.But barium carbonate is as the product of rubber and plastic filler time, because there is stronger wetting ability hydroxyl in the barium carbonate surface; Be hydrophilic oleophobic property, and the polarity difference between the organic polymer is bigger, consistency is bad; Itself be prone to reunite, therefore must carry out suitable surface treatment it.The surface of inorganic powder is through after the modification, and remarkable change all can take place a series of character such as its absorption, wetting, dispersion, thereby the mechanical property of its bonding force, bonding strength and matrix material and physical function all will be strengthened significantly.Inorganic powder modification commonly used can be divided into dry method and wet method: wet-process modifiedly exist the properties-correcting agent loss, need problems such as aftertreatment, cost rising; Dry modification process is simple, does not have the properties-correcting agent loss basically, and modification time is short, effective.
Summary of the invention
The object of the invention is intended to overcome above-mentioned deficiency of the prior art; Through barium carbonate is carried out surface modification; A kind of preparation method of hydrophobicity barium carbonate is provided; Make hydrophobicity barium carbonate (being the modification barium carbonate) and have consistency preferably, can strengthen the thermal property and the mechanical property of bonding force, bonding strength and matrix material with organic polymer.
Content of the present invention is: a kind of preparation method of hydrophobicity barium carbonate; It is characterized in that: get barium carbonate, get the properties-correcting agent of barium carbonate weight 0.1%~20%; With barium carbonate mix with properties-correcting agent, under 50 ℃~170 ℃ temperature stirring reaction (coating) 5~120min, promptly make hydrophobicity barium carbonate (or claim modification barium carbonate);
Said properties-correcting agent can be stearic acid or aluminate coupling agent.
In the content of the present invention: said barium carbonate can be natural magnesium barium (for example: any one witherite etc.) or in the synthetic barium carbonate.
In the content of the present invention: the said hydrophobicity barium carbonate that makes can be used as the packing material of plastics, rubber or coating.
Compared with prior art, the present invention has following characteristics and beneficial effect:
(1) adopts the present invention; During stearic acid modified barium carbonate; Can form unimolecular layer at the barium carbonate microparticle surfaces coats; (-COOH) bonding OH) can take place to carboxyl in the stearic acid molecule in the hydroxyl (-with the absorption of barium carbonate microparticle surfaces; Again because the mutual winding of long chain hydrocarbon groups; Consequently the barium carbonate microparticle surfaces is coated by the stearic acid unimolecular layer, and the barium carbonate microparticle surfaces is organised; During aluminate coupling agent modification barium carbonate, the lip-deep hydroxyl reaction of monoalkoxy in the aluminate coupling agent and barium carbonate forms chemical bonding, and two other organic long-chain and polymer molecule twine, and so just polymkeric substance and filler are combined closely;
(2) adopt the present invention, stearic acid is a kind of auxiliary agent commonly used in plastics industry, and fusing point is suitable, and raw material is easy to get, and human body is not had any toxic action, and low price, and production technique is easy to promotion and implementation, and is pollution-free; Aluminate coupling agent has that performance is good, look shallow, flavor is little, need not thinner, advantage such as easy to use, cheap;
(3) preparation technology of the present invention is simple, and operation is easy, easily operation, and materials such as the hydrophobicity barium carbonate that makes (being the modification barium carbonate) can filled plastics, rubber, coating have a extensive future, and are practical.
Embodiment
Embodiment given below intends so that the present invention is described further; But can not be interpreted as it is restriction to protection domain of the present invention; The person skilled in art to some nonessential improvement and adjustment that the present invention makes, still belongs to protection scope of the present invention according to the content of the invention described above.
Embodiment 1:
The stearic acid of 1.5g is put into the 250ml there-necked flask; Then there-necked flask is placed water bath with thermostatic control; Load onto reflux condensate device; Be heated to 80 ℃ afterwards, add 100g rapidly through pretreated industrial potassium titanate, behind the stirring reaction 30min; The oven dry of taking-up sample; Promptly obtain the modified industry barium carbonate powder, activation index>99%, contact angle 41 ° before by modification are brought up to 125 °.Barium carbonate is after stearic acid modified, and powder granule disperses more even, has effectively improved the agglomeration of powder, volume center particle diameter d 50Reduce to 4.19 μ m by 4.56 μ m, sample was at 1706cm after infrared spectroscopic study showed modification -1The charateristic avsorption band of C=O key disappears 1451cm among the stearic acid carboxyl-COOH of place -1The absorption peak at place is widened, at 1574cm -1Stearate carboxylate anion (CH possibly appear 3(CH 2) 16The absorption bonding takes place in C=O key absorption peak COO-), stearic acid on barium carbonate surface, form new chemical bond, the modification barium carbonate by hydrophilic become hydrophobic.
Embodiment 2
The aluminate coupling agent of 1.5g is put into the 250ml there-necked flask; Then there-necked flask is placed constant temperature oil bath; Load onto reflux condensate device; Be heated to 120 ℃ afterwards, add 100g rapidly through pretreated industrial potassium titanate, behind the stirring reaction 20min; The oven dry of taking-up sample; Promptly obtain the modified industry barium carbonate powder, activation index>98%, it is 112 ° that contact angle 41 ° before by modification are brought up to.Infrared spectroscopic study shows that wave number is 3436cm -1And 1631cm -1The absorption peak at place is respectively hydroxyl stretching vibration and flexural vibration peak, and compares before the modification, and the hydroxyl characteristic peak obviously strengthens, and shows the barium carbonate surfactivity height after the modification; At 2922cm -1And 2852cm -1CH has appearred in the place 3And CH 2Deng the characteristic peak of organic group, this shows and successfully organism has been connected to the barium carbonate particle surface, and aluminate coupling agent on the barium carbonate surface absorption bonding takes place, and forms new chemical bond, the modification barium carbonate by hydrophilic become hydrophobic.
Embodiment 3:
A kind of preparation method of hydrophobicity barium carbonate; Be: get barium carbonate, get the properties-correcting agent of barium carbonate weight 0.1%; With barium carbonate mix with properties-correcting agent, under 50 ℃ of temperature stirring reaction (coating) 120min, promptly make hydrophobicity barium carbonate (or claim modification barium carbonate).
Embodiment 4:
A kind of preparation method of hydrophobicity barium carbonate is: get barium carbonate, get the properties-correcting agent of barium carbonate weight 20%, with barium carbonate mix with properties-correcting agent, under 170 ℃ of temperature stirring reaction (coating) 5min, promptly make hydrophobicity barium carbonate (or claim modification barium carbonate).
Embodiment 5:
A kind of preparation method of hydrophobicity barium carbonate; Be: get barium carbonate, get the properties-correcting agent of barium carbonate weight 10%; With barium carbonate mix with properties-correcting agent, under 110 ℃ of temperature stirring reaction (coating) 60min, promptly make hydrophobicity barium carbonate (or claim modification barium carbonate).
Embodiment 6:
A kind of preparation method of hydrophobicity barium carbonate; Be: get barium carbonate, get the properties-correcting agent of barium carbonate weight 2%; With barium carbonate mix with properties-correcting agent, under 50 ℃~110 ℃ temperature stirring reaction (coating) 40min, promptly make hydrophobicity barium carbonate (or claim modification barium carbonate).
Embodiment 7-13:
A kind of preparation method of hydrophobicity barium carbonate; Be: get barium carbonate, get the properties-correcting agent of barium carbonate weight 0.1%~20%; With barium carbonate mix with properties-correcting agent, under 50 ℃~170 ℃ temperature stirring reaction (coating) 5~120min, promptly make hydrophobicity barium carbonate (or claim modification barium carbonate);
The concrete weight percent consumption of properties-correcting agent sees the following form 1 among each embodiment:
Table 1:
Figure 2011102414737100002DEST_PATH_IMAGE002
In the table 1: the data of properties-correcting agent delegation " 0.5 " are promptly represented " getting the properties-correcting agent of barium carbonate weight 0.5% ", and the rest may be inferred for other.
In the foregoing description 3-13: said properties-correcting agent can be that (for example: manufacturing enterprise is aluminate coupling agent F-1, the aluminate coupling agent F-2 of the Chongqing safe chemical industry of good generation company limited production and sales for stearic acid or aluminate coupling agent; Aluminate coupling agent HY-1108, the aluminate coupling agent HY-988 of the production and sales of Hangzhou Jesse's card chemical industry company limited; The aluminate coupling agent AL-822 of cloud chemical industry company limited production and sales etc. is opened in the Guangzhou).
In the foregoing description 3-13: said barium carbonate can be natural magnesium barium (for example: any one witherite etc.) or in the synthetic barium carbonate.
Said raw material in content of the present invention and the foregoing description is existing marketable material, and the consumption unit of the feed composition that indicates especially is not the weight part (can all be gram or kilogram etc.) with adjacent other component same units; In the percentage that is adopted, do not indicate especially, be weight percent.
In the foregoing description: the processing parameter in each step (temperature, time etc.) and each amounts of components numerical value etc. are scope, and any point is all applicable.
The hydrophobicity barium carbonate that the foregoing description makes can be used as the packing material of plastics, rubber or coating.
The not concrete same prior art of narrating of technology contents in content of the present invention and the foregoing description.
The invention is not restricted to the foregoing description, content of the present invention is said all can implement and have said good result.

Claims (3)

1. the preparation method of a hydrophobicity barium carbonate is characterized in that: get barium carbonate, get the properties-correcting agent of barium carbonate weight 0.1%~20%, with barium carbonate mix with properties-correcting agent, under 50 ℃~170 ℃ temperature stirring reaction 5~120min, promptly make the hydrophobicity barium carbonate;
Said properties-correcting agent is stearic acid or aluminate coupling agent.
2. by the preparation method of the described hydrophobicity barium carbonate of claim 1, it is characterized in that: said barium carbonate is any one in natural magnesium barium or the synthetic barium carbonate.
3. by the preparation method of claim 1 or 2 described hydrophobicity barium carbonates, it is characterized in that: the said hydrophobicity barium carbonate that makes is as the packing material of plastics, rubber or coating.
CN2011102414737A 2011-08-22 2011-08-22 Method for preparing hydrophobic barium carbonate Pending CN102352132A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102675927A (en) * 2012-05-10 2012-09-19 西南科技大学 Preparation method of hydrophobic aluminum phosphate

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1872918A (en) * 2006-06-27 2006-12-06 上海大学 Oleophilic modificatioon method for tiny inorganic Nano powder
CN101768290A (en) * 2010-01-25 2010-07-07 西南科技大学 Modified phosphorous slag used as plastic filler and preparation method thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1872918A (en) * 2006-06-27 2006-12-06 上海大学 Oleophilic modificatioon method for tiny inorganic Nano powder
CN101768290A (en) * 2010-01-25 2010-07-07 西南科技大学 Modified phosphorous slag used as plastic filler and preparation method thereof

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102675927A (en) * 2012-05-10 2012-09-19 西南科技大学 Preparation method of hydrophobic aluminum phosphate

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Application publication date: 20120215