CN109738257A - A kind of preparation method of fine coal coal petrography mating plate - Google Patents

A kind of preparation method of fine coal coal petrography mating plate Download PDF

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Publication number
CN109738257A
CN109738257A CN201910150684.6A CN201910150684A CN109738257A CN 109738257 A CN109738257 A CN 109738257A CN 201910150684 A CN201910150684 A CN 201910150684A CN 109738257 A CN109738257 A CN 109738257A
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coal
mating plate
sample
preparation
coal sample
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CN201910150684.6A
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李丹丹
李茂森
杨毅
李娜
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Shandong University of Science and Technology
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Shandong University of Science and Technology
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Abstract

The invention discloses a kind of preparation methods of fine coal coal petrography mating plate, belong to the preparation technical field of rock mating plate.It is chosen a certain amount of coal sample first and is crushed, and sieve is crossed, and guarantees that coal sample weight of the granularity less than 0.1mm is no more than the 10% of total coal sample weight;100~200g of air-dried sample that granularity is less than 1mm is weighed, and it is spare to 10~20g by its division using heap to mix quartering;Then binder, curing agent, promotor and defoaming agent are mixed, resin liquid is made;After mold molding, freeze-day with constant temperature, fine coal coal petrography mating plate is made.The present invention solves bubble problem present in the polished grain mount being difficult to avoid that in traditional technology, and the quality and utilization efficiency of mating plate are improved using the addition of defoaming agent.The present invention can make full use of material, discard remaining sillar or landwaste using exploitation, and for certain Valuable Minerals, advantage of the invention just apparent can be showed.

Description

A kind of preparation method of fine coal coal petrography mating plate
Technical field
The present invention relates to the preparation technical fields of rock mating plate, and in particular to a kind of preparation method of fine coal coal petrography mating plate.
Background technique
Fine coal mating plate: the also known as cementing mating plate of coal grain or polished grain mount are to be studied and special to coal under reflected light A kind of coal grain mating plate.Advantage is that coal consumption is few and representative relatively strong, is ground conveniently.In microscope viewed in reflected light fine coal light Piece, the features such as according to the reflected colour of coal, protrusion, form and blastema structure, can carry out the quantitative statistics of maceral in coal, The reflectivity and degree of oxidation etc. of comparison and measurement coal.In petrology, by the methods of mineralogy, petrology, chalcography, In conjunction with microscopic observation, to the mineralogical composition of ore and country rock, ore texture, paragenetic association of minerals and genesis sequence, close Mine Alteration Feature of Country Rock, secondary variation etc. are studied, to determine the mineral species of rock or ore, analysis geological structure, pushing away Disconnected mineral deposit generate geological conditions, understand ore processing technical performance and divide ore natural type etc. the data that provides according to According to.
Describe two kinds of method for making sample in GB/T 16773-1997 " coal petrography analysis sample preparation methods ": 1. hot glue methods, 2. cold glue method.Hot glue method specific steps are as follows: it is viscous to dial in bottom by coal sample and binder volume ratio 2:1 feeding by a. after blending uniformly Have in the endless metal mold of paper;B. the mold equipped with coal and binder mixtures is put into cyclic annular electric heater and is heated, mould Temperature is not to be exceeded 100 DEG C in having, and is stirred continuously until binder melts completely;C. the mold equipped with mixture is put into rapidly Pressurize 3.5MPa in pointing machine, stops about 30s, takes out briquet, number;D. mold and tool are cleared up in time.Cold glue method specifically walks Suddenly are as follows: weigh coal sample 10g and pour into cold glue mold slots, the unsaturated polyester resin prepared is given in each coal sample and pours into 7g, side Bevelling stirring, mixes coal glue uniformly, and stirring to glue retrogradation stops stirring, place about 2h to when can prevent the sinking of coal grain, to It is put into the insulating box not higher than 60 DEG C after bubble discharge and is consolidated into briquet, taken out, number.Wherein cold glue method is due to operating procedure Simply, of less demanding to experimental facilities, to be more widely applied.
It is disclosed in CN 102169061A " a kind of production method of rock sample ", including production mold, melts resin, Merge stone sample, Mold polishing.This method is similar to the cold glue method in GB/T 16773-1997, but epoxy resin is used to need 100 DEG C of heating water bath melt completely to epoxy resin and can just be operated, and this method is more time-consuming and laborious.The mistake of moulded products Common problem is to be easy to sandwich air in resin in journey, especially when liquid resin and solid are mixed, due to Liquid resin viscosity larger bubble is not easy to be discharged, or even is also difficult completely to eliminate bubble under conditions of applying vacuum.In coal After brick Sample consolidation, since the presence of bubble can cause high risks to subsequent operation: bubble, which exists, will lead to briquet sample knot Structure intensity is low, easy fragmentation during sanding and polishing;When observing under the microscope, there are bubbles will affect corresponding region for burnishing surface Intensity of light reflection so that briquet surface utilisation is not high, to influence the accuracy of experiment progress and experimental result.
Currently, part bubble can only be removed using standing or beating, but the effect is unsatisfactory.GB/T 16773—1997 In cold glue method also clear stipulaties " stirring to glue retrogradation to when can prevent the coal grain from sinking, stopping stirring, placement about 2h ", this It will certainly delay test progress.
In the prior art, there are no the effective measures of bubble in quick removal briquet, traditional method time and effort consuming and Effect is undesirable, if can solve the problem of bubble in briquet, certainly will carry out great convenience for the observation band of mating plate in petrology, The labor intensity for greatly reducing experimenter, improves experiment progress.And mold and sample demoulding are difficult, it is difficult to separate.
Summary of the invention
In order to solve above-mentioned defect existing in the prior art, the invention proposes a kind of preparation sides of fine coal coal petrography mating plate Method, this method have determined the type and optimum additive amount of defoaming agent, bubble formation have been avoided, to improve sample quality and benefit With rate.
Its technical solution includes:
A kind of preparation method of fine coal coal petrography mating plate, successively the following steps are included:
A prepares fine coal sample, chooses a certain amount of coal sample and is crushed, and crosses sieve, guarantees that granularity is less than the coal sample of 0.1mm Weight is no more than the 10% of total coal sample weight;, 100~200g of air-dried sample that granularity is less than 1mm is weighed, and mix using heap Quartering is spare to 10~20g by its division;
B prepares resin liquid, and by binder, curing agent, promotor and defoaming agent, 100:4:4:2 is carried out according to the weight ratio Resin liquid is made in mixing;
The molding of c mold sprays release agent in mould inner surface, weighs a certain amount of coal sample and pour into mold slots, and will step Resin liquid obtained by rapid b is added to the mold slots equipped with coal sample, stirring while adding, and stirring is to glue retrogradation and can prevent coal sample Stop stirring when sinking;
Mold after molding obtained by step c is put into insulating box and consolidates by d freeze-day with constant temperature, temperature≤60 DEG C of insulating box, To obtain the final product;
The defoaming agent uses the styrene solution of organic silicone defoaming agent, the quality of organic silicone and styrene solution Compare 1:1.
As a preferred solution of the present invention, in step b, the binder is unsaturated polyester resin, described Curing agent is the mixed solution of cyclohexanone peroxide and dibutyl ester, and the promotor is the styrene of the quality of liquid containing cobalt soap 6% Solution.
As another preferred embodiment of the invention, the weight proportion of the cyclohexanone peroxide and dibutyl ester is 1:1.
Further, in step c, release agent is polyurethane water-based release agent, wherein each raw material forms by weight percentage Are as follows: emulsifying wax liquid: 10%~15%;Methyl-silicone oil emulsion: 15%~20%;Modified silicon oil emulsion: 5%~8%;Deionization Water: 50%~55%;Emulsifier: 4.5%~6%;Preservative: 0.3%~0.5%.
Advantageous effects brought by the present invention are as follows:
Compared with prior art, gas present in the polished grain mount being difficult to avoid that in traditional technology is solved using the present invention Problem is steeped, the quality and utilization efficiency of mating plate are improved using the addition of defoaming agent.The method of the present invention is cured, and can go on smoothly Grinding and polishing, and mix uniform.The rock that the present invention can solve certain Special Categories is difficult to the problem of completely sampling, In this way, it is only necessary to which several blocks of rocks of very little just can be carried out test.Secondly, the present invention can make full use of material, using exploitation Remaining sillar or landwaste are discarded, for certain Valuable Minerals, advantage of the invention just apparent can be showed.In addition, Method of the invention is compared with the traditional method, and is convenient in demoulding, and the speed of sample preparation is fast, and product quality is higher, more practical simplicity.
Detailed description of the invention
The present invention will be further described with reference to the accompanying drawing:
Fig. 1 is preparation technology flow chart of the present invention.
Specific embodiment
The invention proposes a kind of preparation methods of fine coal coal petrography mating plate, in order to make advantages of the present invention, technical solution more Add clear, clear, elaborates combined with specific embodiments below to the present invention.
Raw material needed for the present invention can be bought by commercial channel and be obtained.
Release agent of the present invention preferentially selects polyurethane water-based release agent, and the group of each raw material weight percentage is grouped as: emulsification Wax liquor: 10%~15%;Methyl-silicone oil emulsion: 15%~20%;Modified silicon oil emulsion: 5%~8%;Deionized water: 50%~ 55%;Emulsifier: 4.5%~6%;Preservative: 0.3%~0.5%.This aqueous release agent, is mainly used in polyurethane system It is release after product production process moulding by casting, give most polyurethane moulded good stripping results.Its main feature is that the product is with water For dispersed phase, the hydrotrope of formation had both had the function of demoulding polyurethane foam, and but also with biological degradability, VOC free etc. has Evil substance generates, and the feature of environmental protection is strong;And water is as diluent, pollution-free to be easy to get, low cost.
Embodiment 1:
As shown in connection with fig. 1.
Step 1: stock
Choosing coal, binder, curing agent, promotor, defoaming agent and release agent is raw material;
Step 2: the preparation of fine coal sample
Coal sample pulverizer or mortar are crushed first, it is then broken by sieving repeatedly and repeatedly to sieve upper matchmaker's sample, until Completely by testing sieve, the coal sample weight less than 0.1mm is made to be no more than 10%.Weigh the air-dried sample that granularity is less than 1mm 100~200g mixes quartering with heap its division is spare to 10~20g.
Step 3: the preparation of resin liquid
Unsaturated polyester resin, curing agent [cyclohexanone peroxide and dibutyl ester solution (1:1)], (cobalt soap liquid exists promotor 6% solution in styrene) and defoaming agent is by weight ratio, weight ratio 100:4:4:2.Defoaming agent is defoamed using organic silicone The styrene solution of agent, the two mass ratio 1:1, dissolubility are good, easy to use.
Step 4: mold forms
Firstly, spraying release agent in mould inner surface;Then, it weighs coal sample 10g to pour into cold glue mold slots, by what is prepared Resin liquid mixes coal glue uniformly to 7g, the stirring of side bevelling is poured into each coal sample, and stirring to glue retrogradation is to can prevent coal When grain sinks, stop stirring.
Step 5: freeze-day with constant temperature
It is put into the insulating box not higher than 60 DEG C and is consolidated into briquet, take out, number.
Comparative example 1:
Step 1: stock
Choosing coal, binder, curing agent, promotor, defoaming agent and release agent is raw material;
Step 2: the preparation of fine coal sample
Coal sample pulverizer or mortar are crushed first, it is then broken by sieving repeatedly and repeatedly to sieve upper matchmaker's sample, until Completely by testing sieve, the coal sample weight less than 0.1mm is made to be no more than 10%.Weigh the air-dried sample that granularity is less than 1mm 100~200g mixes quartering with heap its division is spare to 10~20g.
Step 3: the preparation of resin liquid
Unsaturated polyester resin, curing agent [cyclohexanone peroxide and dibutyl ester solution (1:1)], (cobalt soap liquid exists promotor 6% solution in styrene) and defoaming agent is by weight ratio, weight ratio 100:4:4:2.Defoaming agent is defoamed using organic silicone The styrene solution of agent, the two mass ratio 1:1, dissolubility are good, easy to use.
Step 4: mold forms
Firstly, spraying release agent in mould inner surface;Then, it weighs coal sample 10g to pour into cold glue mold slots, by what is prepared Resin liquid mixes coal glue uniformly to 10g, the stirring of side bevelling is poured into each coal sample, and stirring to glue retrogradation is to can prevent When coal grain sinks, stop stirring.
Step 5: freeze-day with constant temperature
It is put into the insulating box not higher than 60 DEG C and is consolidated into briquet, take out, number.
It is demonstrated experimentally that using the styrene solution of organic silicone defoaming agent as defoaming agent, antifoaming speed is fast, the foam inhibition time Length, dosage are few.Surface tension is low, disperses in system conducive to the brokenly bubble factor.There is wetting action to substrate, is not likely to produce flake. This product is nontoxic, odorlessness, is conducive to production safety.
It uses for reference the prior art and can be realized in the above-mentioned part that do not address.
It should be noted that any equivalent way that those skilled in the art are made under the introduction of this specification, or Obvious variant should all be within the scope of the present invention.

Claims (4)

1. a kind of preparation method of fine coal coal petrography mating plate, which is characterized in that successively the following steps are included:
A prepares fine coal sample, chooses a certain amount of coal sample and is crushed, and crosses sieve, guarantees that granularity is less than the coal sample weight of 0.1mm No more than the 10% of total coal sample weight;100~200g of air-dried sample that granularity is less than 1mm is weighed, and mixes four points using heap Method is spare to 10~20g by its division;
B prepares resin liquid, and by binder, curing agent, promotor and defoaming agent, 100:4:4:2 is mixed according to the weight ratio It closes, resin liquid is made;
The molding of c mold sprays release agent in mould inner surface, weighs a certain amount of coal sample and pour into mold slots, and by step b institute It obtains resin liquid to be added to the mold slots equipped with coal sample, stirring while adding, stirring is to glue retrogradation and can prevent coal sample from sinking When stop stirring;
Mold after molding obtained by step c is put into insulating box and consolidates by d freeze-day with constant temperature, temperature≤60 DEG C of insulating box, i.e., ?;
The defoaming agent uses the styrene solution of organic silicone defoaming agent, the mass ratio 1 of organic silicone and styrene solution: 1。
2. a kind of preparation method of fine coal coal petrography mating plate according to claim 1, it is characterised in that: described in step b Binder is unsaturated polyester resin, and the curing agent is the mixed solution of cyclohexanone peroxide and dibutyl ester, the rush It is the styrene solution of the quality of liquid containing cobalt soap 6% into agent.
3. a kind of preparation method of fine coal coal petrography mating plate according to claim 2, it is characterised in that: the peroxidating ring The weight proportion of ketone and dibutyl ester is 1:1.
4. a kind of preparation method of fine coal coal petrography mating plate according to claim 1, it is characterised in that: in step c, release agent For polyurethane water-based release agent, wherein each raw material forms by weight percentage are as follows: emulsifying wax liquid: 10%~15%;Methyl-silicone oil Lotion: 15%~20%;Modified silicon oil emulsion: 5%~8%;Deionized water: 50%~55%;Emulsifier: 4.5%~6%; Preservative: 0.3%~0.5%.
CN201910150684.6A 2019-02-28 2019-02-28 A kind of preparation method of fine coal coal petrography mating plate Pending CN109738257A (en)

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CN113092467A (en) * 2020-11-06 2021-07-09 长江大学 Intelligent microscopic identification quantitative system for whole rock slide
CN113776910A (en) * 2021-09-14 2021-12-10 中海油能源发展股份有限公司 Coal sample preparation method for measuring coal rock expansion prevention rate of liquid by dilatometer method

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Publication number Priority date Publication date Assignee Title
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CN113776910A (en) * 2021-09-14 2021-12-10 中海油能源发展股份有限公司 Coal sample preparation method for measuring coal rock expansion prevention rate of liquid by dilatometer method
CN113776910B (en) * 2021-09-14 2024-05-17 中海油能源发展股份有限公司 Preparation method of coal sample for measuring anti-swelling rate of liquid to coal and rock by dilatometer method

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Application publication date: 20190510