CN103468149A - Chlorinated rare earth polishing powder and production method thereof - Google Patents

Abstract

The invention relates to chlorinated rare earth polishing powder and a production method thereof. The method mainly comprises the following steps: precursor generation and block amino silicon oil generation. The block amino silicon oil produced by the method disclosed by the invention does not generate solid salt due to the fact that no concentrated sulfuric acid or sodium bicarbonate is used. Thus, the possibility of environmental pollution is reduced. In addition, the entire production process just needs two days; the production period is shortened; the production time is greatly saved.

Description

A kind of rare earth chloride polishing powder and production method

Technical field

The present invention relates to field of surface treatment, specifically a kind of rare earth chloride polishing powder and production method.

Background technology

The relation of the mankind and chemical industry is very close, in the modern life, almost all be unable to do without Chemicals whenever and wherever possible, from material lifes such as clothing, food, shelter, row to cultural lives such as culture and arts, amusements, all needs Chemicals to serve for it.Some Chemicals, in human development history, plays epoch-making vital role.Their production and application, even representing certain historical stage of human civilization.

At present, for the textile fabric feel, processing is mainly amido silicon oil and the amino block amido silicon oil that is distributed in main chain that amino is distributed in side chain.While using the amino amido silicon oil that is distributed in side chain to process as feel, needing first this type of amido silicon oil to be added tensio-active agent emulsification to form stable emulsion could use; And the amino block amido silicon oil that is distributed in main chain due in structure with hydrophilic radical, while using as the feel treatment agent without separately adding tensio-active agent just can form stable emulsion.In addition, while using as the feel treatment agent, the block amido silicon oil that amino is distributed in main chain is compared the amido silicon oil that amino is distributed in side chain following advantage: soft, level and smooth, fluffy feel is outstanding, and usage quantity is little.

Because routine is produced block amido silicon oil employing three-step approach, the first step: methyl cyclosiloxane and tetramethyl-dihydro base sily oxide under the effect as catalyzer, carry out balanced reaction at the vitriol oil, after the reaction certain hour, add in sodium bicarbonate and the vitriol oil, filter, obtain holding containing hydrogen silicone oil; Second step: add glycidyl allyl ether and chloroplatinic acid catalyst in the end containing hydrogen silicone oil, react under certain temperature, after reaction finishes, the reactant that the intensification vacuum removal is unnecessary, obtain end ring oxygen silicone oil; The 3rd step: end ring oxygen silicone oil is reacted under solvent with polyetheramine, obtains the block amido silicon oil.Can produce a large amount of solid salts with the vitriol oil in sodium bicarbonate in the first step, can't recycle, may cause environmental pollution, and whole production process needs about 3 days.Also do not have at present a kind of production technique simple, can not impact environment, and the production method of mass production block amido silicon oil with short production cycle.

Summary of the invention

The present invention, just for above technical problem, provides a kind of production technique simple, can not impact environment, and the production method of mass production block amido silicon oil with short production cycle.

The present invention is achieved through the following technical solutions.

A kind of rare earth chloride polishing powder, be 46～54% containing the rare earth composition weight percent, and surplus is oxalic acid, and the principal element content in rare earth meets following the requirement: CaO+MgO≤3%, CeO>=60%, Nd ₂o ₃>=0.2%, La ₂o ₃>=28%, Pr ₂o ₃>=5%.

A kind of rare earth chloride polishing powder and production method mainly comprise the following steps:

One, hybrid reaction, take rare earth, calculates consumption of oxalic acid, oxalic acid fully mixed to standing the reaction with rare earth;

Two, roasting, be heated to 900～950 ℃ by rare earth and oxalic acid mixture and carry out preroasting 1 hour, then rare earth and oxalic acid mixture reheated and be warming up to 1100～1150 ℃ of roastings 5 hours;

Three, pulverize and sieve, the material after roasting is down to room temperature, pulverized, then sieve, the oversize material of failing to sieve is pulverized again;

Four, purged and packed, cleaned the material after sieving, and then dries, then be down to room temperature and packed.

It is consistent that the polishing powder that adopts the method for the invention to produce has the micro mist epigranular,, containing mechanical impurity, do not have higher dispersiveness and absorption, and polishing efficiency is high, and have good wetting property that the characteristics such as suspension are arranged with water.Applicable to the high-precision optical polishing.And, because the present invention has adopted re-baking, reaction process is more thorough.

Embodiment

Below in conjunction with specific embodiment, the invention will be further described.

Embodiment 1:

One, hybrid reaction, take rare earth 500Kg, and oxalic acid 500Kg fully mixes oxalic acid with rare earth, the standing reaction;

Two, roasting, be heated to 930 ℃ by rare earth and oxalic acid mixture and carry out preroasting 1 hour, then rare earth and oxalic acid mixture reheated and be warming up to 1130 ℃ of roastings 5 hours;

Three, pulverize and sieve, the material after roasting is down to room temperature, pulverized, then sieve, the oversize material of failing to sieve is pulverized again;

Four, purged and packed, cleaned the material after sieving, and then dries, then be down to room temperature and packed.

Embodiment 2:

One, hybrid reaction, take 460Kg, and oxalic acid 540Kg fully mixes oxalic acid with rare earth, the standing reaction;

Two, roasting, be heated to 950 ℃ by rare earth and oxalic acid mixture and carry out preroasting 1 hour, then rare earth and oxalic acid mixture reheated and be warming up to 1150 ℃ of roastings 5 hours;

Three, pulverize and sieve, the material after roasting is down to room temperature, pulverized, then sieve, the oversize material of failing to sieve is pulverized again;

Four, purged and packed, cleaned the material after sieving, and then dries, then be down to room temperature and packed.

Embodiment 3:

One, hybrid reaction, take 540Kg, and oxalic acid 460Kg fully mixes oxalic acid with rare earth, the standing reaction;

Two, roasting, be heated to 900 ℃ by rare earth and oxalic acid mixture and carry out preroasting 1 hour, then rare earth and oxalic acid mixture reheated and be warming up to 1100 ℃ of roastings 5 hours;

Three, pulverize and sieve, the material after roasting is down to room temperature, pulverized, then sieve, the oversize material of failing to sieve is pulverized again;

Four, purged and packed, cleaned the material after sieving, and then dries, then be down to room temperature and packed.

Through experiment test, above two kinds of specific embodiments all can be produced the polishing powder applicable to the high-precision optical polishing.When oxalic acid content increases, need suitably to improve maturing temperature in the reasonable scope.

It is consistent that the polishing powder that adopts the method for the invention to produce has the micro mist epigranular,, containing mechanical impurity, do not have higher dispersiveness and absorption, and polishing efficiency is high, and have good wetting property that the characteristics such as suspension are arranged with water.Applicable to the high-precision optical polishing.And, because the present invention has adopted re-baking, reaction process is more thorough.

Claims (5)

1. a rare earth chloride polishing powder, be 46～54% containing the rare earth composition weight percent, and surplus is oxalic acid, and the principal element content in rare earth meets following the requirement: CaO+MgO≤3%, CeO>=60%, Nd ₂o ₃>=0.2%, La ₂o ₃>=28%, Pr ₂o ₃>=5%.

2. a kind of rare earth chloride polishing powder according to claim 1, is characterized in that content of rare earth is 50%, and surplus is oxalic acid.

3. a kind of rare earth chloride polishing powder according to claim 1, is characterized in that content of rare earth is 46%, and surplus is oxalic acid.

4. a kind of rare earth chloride polishing powder according to claim 1, is characterized in that content of rare earth is 54%, and surplus is oxalic acid.

5. the production method of a rare earth chloride polishing powder mainly comprises the following steps:

One, hybrid reaction, take rare earth, calculates consumption of oxalic acid, oxalic acid fully mixed to standing the reaction with rare earth;

Two, roasting, be heated to 900～950 ℃ by rare earth and oxalic acid mixture and carry out preroasting 1 hour, then rare earth and oxalic acid mixture reheated and be warming up to 1100～1150 ℃ of roastings 5 hours;

Three, pulverize and sieve, the material after roasting is down to room temperature, pulverized, then sieve, the oversize material of failing to sieve is pulverized again;

Four, purged and packed, cleaned the material after sieving, and then dries, then be down to room temperature and packed.