CN108864382A - A kind of dibutyl phthalate and preparation method for coal mine atomizing de-dusting - Google Patents

A kind of dibutyl phthalate and preparation method for coal mine atomizing de-dusting Download PDF

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Publication number
CN108864382A
CN108864382A CN201810705644.9A CN201810705644A CN108864382A CN 108864382 A CN108864382 A CN 108864382A CN 201810705644 A CN201810705644 A CN 201810705644A CN 108864382 A CN108864382 A CN 108864382A
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dibutyl phthalate
preparation
mentioned
dust
lignosulfonates
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CN201810705644.9A
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CN108864382B (en
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周刚
丁建飞
孙健
高丹红
潘红卫
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Shandong University of Science and Technology
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Shandong University of Science and Technology
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Priority to CN201810705644.9A priority Critical patent/CN108864382B/en
Priority to PCT/CN2018/100451 priority patent/WO2020006817A1/en
Priority to JP2020564935A priority patent/JP7050364B2/en
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F289/00Macromolecular compounds obtained by polymerising monomers on to macromolecular compounds not provided for in groups C08F251/00 - C08F287/00
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K3/00Materials not provided for elsewhere
    • C09K3/22Materials not provided for elsewhere for dust-laying or dust-absorbing

Abstract

The invention discloses a kind of dibutyl phthalates and preparation method for coal mine atomizing de-dusting comprising:The lignosulfonates of 3%-5%, the vinyl acetate of 3%-5%, the 2- acrylamide-2-methyl propane sulfonic of 3%-5%, the initiator of 0.05%-0.1%, the crosslinking agent of 0.02%-0.04%, the antifreezing agent of 0.3%-0.6% and the corrosion inhibiter of 0.2%-0.4%, surplus are water.Using sodium lignin sulfonate as matrix, polymerization reaction is carried out with vinyl acetate, 2- acrylamide-2-methyl propane sulfonic, the polymer of generation had not only maintained the degradable performance of sodium lignin sulfonate, but also the function that droplet can be made to have wetting, bonding.This is used for the spraying dibutyl phthalate of coal mine and surfactant compound is applied in spraying system, the spraying wetability to coal dust can be further increased, droplet is set effectively to be soaked, be wrapped up to dust, substantially increase dust suppression efficiency, reduce dust recycling, and the case where causing secondary pollution after depositing dust appearance can be avoided with natural decomposition.

Description

A kind of dibutyl phthalate and preparation method for coal mine atomizing de-dusting
Technical field
The present invention relates to mines dust-proof, dust suppression field more particularly to a kind of dibutyl phthalate and system for coal mine atomizing de-dusting Preparation Method.
Background technique
With the progress of science and technology, the mechanization of coal mining, the degree of automation are higher and higher, produce in this process Raw dust is also more and more.Mine Dust be seriously endanger downhole production safety and personnel's health major casualty source it One, the harm of coal dust mainly has following several respects:It even explodes first is that spontaneous combustion can occur under certain condition, easily initiation gas Explosion accident;Second is that seriously threatening the physical and mental health of Coal Miners with the increase of respirable dust concentration, it being made to suffer from dirt The probability of tuberculosis and other pulmonary diseases greatly increases;Third is that the dust of underground coal mine can aggravate the mill of underground equipment components Damage causes accuracy of instrument decline or failure;In addition a large amount of dust can reduce the visibility of underground, Yi Fashengyin maloperation and lead Cause the accident of casualties.According to actual measurement, in the case where not taking any measure, the dust concentration of fully mechanized workface is reachable 3000mg/m3More than, the dust concentration of fully-mechanized mining working is more up to 6000mg/m3More than.
Underground coal mine face is in order to prevent and treat the method that dust generally uses atomizing de-dusting, however since coal body itself is hydrophobic Characteristic, water is poor to the wetability of coal dust, it is difficult to reach ideal effect.For coal dust itself difficult the characteristics of soaking, at present Widely applied technology is to add ready-made technical grade surfactant or Surfactant in water to be compounded.But it is this The drawbacks such as that there is dust-laying effects is poor, at high cost for method, toxicity is high, and conventional surfactant is not degradable, large area is answered With also will cause secondary environmental pollution.
Summary of the invention
In view of above-mentioned deficiencies of the prior art, the purpose of the present invention is to provide a kind of increasing profits for coal mine atomizing de-dusting Agent and preparation method improve dust suppression efficiency to reduce the diffusion of dust.
In order to solve the above technical problems, the present invention program includes:
A kind of dibutyl phthalate for coal mine atomizing de-dusting, includes following components by mass percentage:
The lignosulfonates of 3%-5%, the vinyl acetate of 3%-5%, 3%-5% 2- acrylamide -2- methyl Propane sulfonic acid, the initiator of 0.05%-0.1%, the crosslinking agent of 0.02%-0.04%, 0.3%-0.6% antifreezing agent and 0.2%- 0.4% corrosion inhibiter, surplus are water.
The dibutyl phthalate, wherein above-mentioned lignosulfonates are one of sodium lignin sulfonate, calcium lignosulfonate Or mixtures thereof;Above-mentioned initiator is one of sodium peroxide, ammonium persulfate;Crosslinking agent is N-N methylene-bisacrylamide.
The dibutyl phthalate, wherein above-mentioned antifreezing agent is calcium chloride;Corrosion inhibiter is phosphorus carboxylic acid.
A kind of preparation method of above-mentioned dibutyl phthalate comprising following steps:
After dissolving lignosulfonates in water, vinyl acetate is added in step 1, and the temperature of constant temperature stirring instrument is set It is stirred 30 minutes after being set to 60 DEG C, initiator is added into above-mentioned solution again after all dissolutions are sufficiently mixed, it is anti-at 60 DEG C It answers 2 hours, obtains the first solution;
Step 2, then to be added into the first solution 2- acrylamide-2-methyl propane sulfonic and crosslinking agent the reaction was continued 1 small When, obtain final product;
Antifreezing agent and corrosion inhibiter are added into final product, stirs, and adjust pH value, can obtain for step 3 To above-mentioned dibutyl phthalate.
The preparation method, wherein the above-mentioned dibutyl phthalate of preparation carries out being thoroughly mixed spare, dibutyl phthalate again with water With water according to mass ratio be 1:50 ratio is thoroughly mixed.
The preparation method, wherein the pH value in step 3 is 7-8.
The preparation method, wherein above-mentioned lignosulfonates are sodium lignin sulfonate, one in calcium lignosulfonate Or mixtures thereof kind;Above-mentioned initiator is one of sodium peroxide, ammonium persulfate;Crosslinking agent is N-N methylene bisacrylamide acyl Amine.
The preparation method, wherein above-mentioned antifreezing agent is calcium chloride;Corrosion inhibiter is phosphorus carboxylic acid.
A kind of dibutyl phthalate and preparation method for coal mine atomizing de-dusting provided by the invention, utilizes the Strong oxdiative of persulfuric acid Property capture-OH in lignin hydrogen generate primary group of free radicals, primary group of free radicals attack vinyl acetate, 2- acrylamide -2- first The free radical of generation is carried out polymerization reaction, by 2- by the C=C of base propane sulfonic acid and N-N methylene-bisacrylamide in aqueous solution Acrylamide-2-methyl propane sulfonic and vinyl acetate are grafted on sodium lignin sulfonate.The original sulfonic acid of sodium lignin sulfonate Group has preferable absorption property to coal dust, and amide group makes the drop sprayed have certain adhesiveness, ester group to coal dust Enhance the overall structure generated to the wetting ability of coal dust.This dibutyl phthalate and surfactant compound are applied to spraying system In, the surface tension of water is not only reduced, and wetting of the droplet to dust, adhesiving effect can be increased, keeps droplet effective Dust is soaked, adhered to, is wrapped up, dust suppression efficiency is substantially increased, reduces dust recycling.In addition this dibutyl phthalate is with wooden Plain sodium sulfonate is matrix, can natural decomposition, avoid the case where causing secondary pollution after depositing dust appearance.
Detailed description of the invention
Fig. 1 is the flow diagram that dibutyl phthalate is prepared in the present invention.
Specific embodiment
The present invention provides a kind of dibutyl phthalate and preparation method for coal mine atomizing de-dusting, for make the purpose of the present invention, Technical solution and effect are clearer, clear, and the present invention is described in more detail below.It should be appreciated that described herein Specific embodiment is only used to explain the present invention, is not intended to limit the present invention.
The present invention provides a kind of dibutyl phthalates for coal mine atomizing de-dusting, include by mass percentage:3%-5%'s Lignosulfonates, the vinyl acetate of 3%-5%, 3%-5% 2- acrylamide-2-methyl propane sulfonic, 0.05%- 0.1% initiator, the crosslinking agent of 0.02%-0.04%, the antifreezing agent of 0.3%-0.6% and 0.2%-0.4% corrosion inhibiter, Surplus is water.And above-mentioned lignosulfonates are or mixtures thereof one of sodium lignin sulfonate, calcium lignosulfonate;On Stating initiator is one of sodium peroxide, ammonium persulfate;Crosslinking agent is N-N methylene-bisacrylamide.Above-mentioned antifreezing agent is Calcium chloride;Corrosion inhibiter is phosphorus carboxylic acid.
The present invention also provides a kind of preparation method of above-mentioned dibutyl phthalate, as shown in Figure 1 comprising following steps:
After dissolving lignosulfonates in water, vinyl acetate is added in step 1, and the temperature of constant temperature stirring instrument is set It is stirred 30 minutes after being set to 60 DEG C, initiator is added into above-mentioned solution again after all dissolutions are sufficiently mixed, it is anti-at 60 DEG C It answers 2 hours, obtains the first solution;
Step 2, then to be added into the first solution 2- acrylamide-2-methyl propane sulfonic and crosslinking agent the reaction was continued 1 small When, obtain final product;
Antifreezing agent and corrosion inhibiter are added into final product, stirs, and adjust pH value, can obtain for step 3 To above-mentioned dibutyl phthalate.
In order to which the present invention is further described, it is exemplified below more specifically embodiment and is illustrated.
Embodiment 1:
It weighs 2g sodium lignin sulfonate and 4ml vinyl acetate is dissolved in 200ml water, after sufficiently dissolving and stirring 30min, 0.5g ammonium persulfate is added into solution, constant temperature is stirred to react 2 hours at 60 DEG C.2g2- acrylamide-the 2- into solution again Methyl propane sulfonic acid and 0.5gN-N methylene-bisacrylamide are kept for 60 DEG C and continue to be stirred to react 2 hours.After the reaction was completed, Xiang Rong 0.3g calcium chloride and 0.2ml phosphorus carboxylic acid are added in liquid, adjusts pH, 2ml and 0.2g dodecyldimethylammonium hydroxide inner salt is taken to add simultaneously Enter in 1L water and be uniformly mixed, tests correlated performance.
Embodiment 2:
It weighs 2g sodium lignin sulfonate and 4ml vinyl acetate is dissolved in 200ml water, after sufficiently dissolving and stirring 30min, 0.5g ammonium persulfate is added into solution, constant temperature is stirred to react 2 hours at 60 DEG C.4g2- acrylamide-the 2- into solution again Methyl propane sulfonic acid and 0.5gN-N methylene-bisacrylamide are kept for 60 DEG C and continue to be stirred to react 2 hours.After the reaction was completed, Xiang Rong 0.3g calcium chloride and 0.2ml phosphorus carboxylic acid are added in liquid, adjusts PH, 2ml and 0.2g dodecyldimethylammonium hydroxide inner salt is taken to add simultaneously Enter in 1L water and be uniformly mixed, tests correlated performance.
Embodiment 3:
It weighs 2g sodium lignin sulfonate and 4ml vinyl acetate is dissolved in 200ml water, after sufficiently dissolving and stirring 30min, 0.5g ammonium persulfate is added into solution, constant temperature is stirred to react 2 hours at 60 DEG C.6g2- acryloyl is added into solution again Amine -2- methyl propane sulfonic acid and 0.5gN-N methylene-bisacrylamide are kept for 60 DEG C and continue to be stirred to react 2 hours.Reaction is completed Afterwards, 0.3g calcium chloride and 0.2ml phosphorus carboxylic acid are added into solution, adjusts PH, takes 2ml and 0.2g dodecyldimethylammonium hydroxide inner salt It is added in 1L water and is uniformly mixed simultaneously, test correlated performance.
Table 1
As can be seen from the table, 42~55% or so be can only achieve only with clear water atomizing de-dusting efficiency, highest depositing dust Rate is 56.2%, and effect is poor, and the spraying measure efficiency of dust collection for adding dibutyl phthalate can reach 90% or more, up to 93.5%, so that average total dust concentration of working face and averagely dust concentration is exhaled to be down to 51.4mg/m3And 18.8mg/m3, meet drop The needs of dirt.This is because the original sulfonic acid group of sodium lignin sulfonate has preferable absorption property to coal dust, amide group makes Obtaining dibutyl phthalate has certain adhesiveness to coal dust, and ester group enhances the overall structure generated to the wetting ability of coal dust.By this The dibutyl phthalate and surfactant compound spraying for coal mine is applied in spraying system, substantially increases dust suppression efficiency, is reduced Dust recycling.And this dust suppressant is mainly made of natural products, and it is harmless nontoxic, it can voluntarily degrade.
Certainly, described above is only that presently preferred embodiments of the present invention is answered the present invention is not limited to enumerate above-described embodiment When explanation, anyone skilled in the art is all equivalent substitutes for being made, bright under the introduction of this specification Aobvious variant, all falls within the essential scope of this specification, ought to be by protection of the invention.

Claims (8)

  1. It by mass percentage include following components 1. a kind of dibutyl phthalate for coal mine atomizing de-dusting, is characterized in that:
    The lignosulfonates of 3%-5%, the vinyl acetate of 3%-5%, 3%-5% 2- acrylamide -2- methyl-prop sulphur The antifreezing agent and 0.2%- of acid, the initiator of 0.05%-0.1%, the crosslinking agent of 0.02%-0.04%, 0.3%-0.6% 0.4% corrosion inhibiter, surplus are water.
  2. 2. dibutyl phthalate according to claim 1, which is characterized in that above-mentioned lignosulfonates are sodium lignin sulfonate, wood Or mixtures thereof one of quality sulfoacid calcium;Above-mentioned initiator is one of sodium peroxide, ammonium persulfate;Crosslinking agent is N- N methylene-bisacrylamide.
  3. 3. dibutyl phthalate according to claim 1, which is characterized in that above-mentioned antifreezing agent is calcium chloride;Corrosion inhibiter is phosphorus carboxylic acid.
  4. 4. a kind of preparation method of dibutyl phthalate as described in claim 1 comprising following steps:
    After dissolving lignosulfonates in water, vinyl acetate is added in step 1, and the temperature setting by constant temperature stirring instrument is It is stirred 30 minutes after 60 DEG C, initiator is added into above-mentioned solution again after all dissolutions are sufficiently mixed, it is small that 2 are reacted at 60 DEG C When, obtain the first solution;
    Step 2, then into the first solution, the reaction was continued 1 hour for addition 2- acrylamide-2-methyl propane sulfonic and crosslinking agent, obtains To final product;
    Antifreezing agent and corrosion inhibiter are added into final product, stirs, and adjust pH value, can be obtained for step 3 State dibutyl phthalate.
  5. 5. the preparation method according to claim 4, which is characterized in that the above-mentioned dibutyl phthalate of preparation is sufficiently stirred with water again It is 1 that mixing for standby use, dibutyl phthalate and water, which are mixed, according to mass ratio:50 ratio is thoroughly mixed.
  6. 6. the preparation method according to claim 4, which is characterized in that the pH value in step 3 is 7-8.
  7. 7. the preparation method according to claim 4, which is characterized in that above-mentioned lignosulfonates be sodium lignin sulfonate, Or mixtures thereof one of calcium lignosulfonate;Above-mentioned initiator is one of sodium peroxide, ammonium persulfate;Crosslinking agent is N-N methylene-bisacrylamide.
  8. 8. the preparation method according to claim 4, which is characterized in that above-mentioned antifreezing agent is calcium chloride;Corrosion inhibiter is phosphorus carboxylic Acid.
CN201810705644.9A 2018-07-02 2018-07-02 A kind of dibutyl phthalate and preparation method for coal mine atomizing de-dusting Active CN108864382B (en)

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CN201810705644.9A CN108864382B (en) 2018-07-02 2018-07-02 A kind of dibutyl phthalate and preparation method for coal mine atomizing de-dusting
PCT/CN2018/100451 WO2020006817A1 (en) 2018-07-02 2018-08-14 Moistening agent for coal mine spray and dust reduction and preparation method
JP2020564935A JP7050364B2 (en) 2018-07-02 2018-08-14 Moisturizer and preparation method for reducing dust by spraying coal mine

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CN109813849A (en) * 2019-02-14 2019-05-28 中国矿业大学 A method of dust suppression foaming properties are quantitatively evaluated
CN110105920A (en) * 2019-06-04 2019-08-09 中国葛洲坝集团易普力股份有限公司 Green high-efficient mine road dust inhibitor and preparation method thereof
CN112174805A (en) * 2020-11-10 2021-01-05 杭州电化集团有限公司 Production method of sodium acetate capable of not crystallizing at low temperature
CN112459825A (en) * 2020-11-03 2021-03-09 山东科技大学 Mine dust-suppression and explosion-suppression agent, preparation method and application

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CN110105920A (en) * 2019-06-04 2019-08-09 中国葛洲坝集团易普力股份有限公司 Green high-efficient mine road dust inhibitor and preparation method thereof
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CN112174805A (en) * 2020-11-10 2021-01-05 杭州电化集团有限公司 Production method of sodium acetate capable of not crystallizing at low temperature

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