CN103865597B - A kind of nothing discharge production technology of Sulfonates additive - Google Patents
A kind of nothing discharge production technology of Sulfonates additive Download PDFInfo
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- CN103865597B CN103865597B CN201410107818.3A CN201410107818A CN103865597B CN 103865597 B CN103865597 B CN 103865597B CN 201410107818 A CN201410107818 A CN 201410107818A CN 103865597 B CN103865597 B CN 103865597B
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Abstract
The present invention relates to a kind of nothing discharge production technology of Sulfonates additive.Comprise sulfonation, hydrolysis, condensation, neutralization procedure successively, be characterized in: the SO that sulfonation procedure is produced
2waste gas sodium hydroxide solution carries out tail gas absorption, then the absorbing liquid obtained is mixed with certain density sodium hydroxide solution with fresh liquid caustic soda together with water, then this sodium hydroxide solution is joined neutralization procedure uses as raw material.Production technology of the present invention compared with prior art, has the following advantages: 1, non-exhaust emission in production process, environmental friendliness.2, the waste liquid absorbing tail gas is reused for the production of additive, turns waste into wealth.The beneficial effect of production technology of the present invention is to recycle waste resource, solves by producing the environmental pollution brought simultaneously.Through probationary certificate, the Additive Properties that the present invention produces without discharge technology still can meet the means of transportation such as pumping, atomization and combustion requirements, is applicable to the coal sample of different regions.
Description
Technical field
The present invention relates to a kind of nothing discharge production technology of Sulfonates additive.
Background technology
The energy resource structure of China is rich coal, oil-poor, weak breath, and coal accounts for 70% of total energy consumption, and within the period quite grown future, the production of energy based on coal and consumption structure, in China, the change of essence can not occur.Traditional Coal Energy Source utilizes and brings increasingly serious environment contradiction, and the transition therefore realizing coal utilization is imperative." 12 " period China will focus on Development of Coal chemical industry, target be realization from traditional coal chemical industry to Modern Coal-based Chemical, meticulous Coal Chemical Industry upgrade.Modern Coal-based Chemical can solve that traditional coal chemical products are identical, competitiveness is poor, problem of excess production capacity, the problem such as can solve again energy conversion efficiency and comprehensive utilization of resources level is on the low side.New type coal gasification technology, especially Opposed Nozzle Gasifier For Coal Water Slurry, be the leading technology of Modern Coal-based Chemical industry, be also significantly one of basic technology promoting the traditional coal chemical industry levels such as synthetic ammonia, in energy-conserving and environment-protective, coal adaptability etc., there is very outstanding advantage.
Water-coal-slurry technology of preparing is one of key technology of water coal slurry pressure gasification.In water-coal-slurry technology of preparing, slurries additive agent plays vital effect to water-coal-slurry performance, can improve the concentration of water-coal-slurry, rheological characteristic and improve the stability of water-coal-slurry.The investigative technique of external slurries additive agent has been tending towards ripe, especially the scientific research personnel of the U.S., Japan has developed the additive of a large amount of function admirable, as NSF(naphthalene sulfonate polymer), PSS(poly styrene sulfonate), this two classes additive suitability for industrialized production all.Nippon grease company, Kao company, Lion company and Com company are to the research of dedicated water slurry additive system in the extreme.In recent years, China's slurries additive agent makes some progress at everyways such as developmental research, pulping technique, accumulating and burn application, and progressively steps into commercialization stage.But lay particular emphasis on the research of additive at present and probe into the impact of medicament on coal grain paste-forming properties, the research work of slurries additive agent itself is done less, to the design studies phoenix feathers and unicorn horns especially of additive synthesis technique.
Summary of the invention
The object of this invention is to provide a kind of produce Sulfonates additive without discharge technology, whole technique can realize producing without the green of outer discharge, solve waste gas discharge of wastewater contaminated environment in traditional handicraft, waste resource problem.
A nothing discharge production technology for Sulfonates additive, comprise sulfonation, hydrolysis, condensation, neutralization procedure successively, its special feature is: SO sulfonation procedure produced
2waste gas sodium hydroxide solution carries out tail gas absorption, then the absorbing liquid obtained is mixed with certain density sodium hydroxide solution with fresh liquid caustic soda together with water, then this sodium hydroxide solution is joined neutralization procedure uses as raw material.
Wherein tail gas absorption specifically refers to SO
2waste gas mass fraction is sodium hydroxide solution spray-absorption in acid gas absorption tower of 8 ~ 10%, the spent lye obtained first determines the concentration of wherein NaOH, when in the spent lye obtained, NaOH mass fraction is 1 ~ 5%, this spent lye is back to use and joins alkali groove, with mass fraction be 32% liquid caustic soda or mass fraction be 32% liquid caustic soda and water be mixed with the sodium hydroxide solution that mass fraction is 16 ~ 25%.
Wherein measuring spent lye specifically adopts Potassium Hydrogen Phthalate titration to determine the concentration of sodium hydroxide solution.
Further, the formaldehyde exhaust-gas water that condensation step produces is carried out tail gas absorption, when formaldehyde mass fraction is 1 ~ 6% in the formalin obtained, this formalin can be joined in hydrolysing step and use as raw material.
Wherein tail gas absorption specifically refers to formaldehyde exhaust-gas water spray-absorption in acid gas absorption tower; In the absorbing liquid obtained, the content assaying method of formaldehyde is: absorbing liquid and excessive neutral sodium sulfite solution reaction, with the titration of sulfuric acid standard liquid.
Further, comprise the steps:
(1) sulfonation: sulfonating reaction raw material is carbolineum and mass fraction is the concentrated sulfuric acid of 98%, the two mass ratio is 1:0.6 ~ 0.9, first carbolineum is added in reactor A and be preheated to 100 ~ 120 DEG C, then by flowmeter, the concentrated sulfuric acid is dropped in reactor A, control rate of addition is 60 ~ 70kg/min, afterwards the temperature of reactor A is risen to 120 ~ 140 DEG C, insulation reaction 1 ~ 3h;
By the SO produced in said process
2waste gas mass fraction is sodium hydroxide solution spray-absorption in acid gas absorption tower of 8 ~ 10%, the spent lye obtained after absorption first determines the concentration of wherein NaOH, again this spent lye is back to use the sodium hydroxide solution that the liquid caustic soda of liquid caustic soda or the mass fraction 32% of joining alkali groove and mass fraction 32% and water are mixed with mass fraction 16 ~ 25%, then this sodium hydroxide solution is joined in neutralization procedure uses as raw material;
(2) be hydrolyzed: sulfonation procedure terminates rear stopping heating, be cooled to 100 ~ 120 DEG C, while cooling by mass fraction be 1 ~ 6% formaldehyde absorbent add in reactor, total quality of material ratio that this formaldehyde absorbent and step (1) obtain is 1:1.5 ~ 2, at 100 ~ 120 DEG C of hydrolysis 0.5 ~ 1.5h;
(3) condensation: the material after hydrolysis is delivered in reactor B, still temperature control is at 50 ~ 70 DEG C, the formalin of mass fraction 36.7% ~ 37.4% is added dropwise in reactor B, total quality of material that this formalin and step (2) obtain is than being 1:6 ~ 7, rate of addition is 10 ~ 16kg/min, temperature rises to 80 ~ 90 DEG C subsequently, insulation 1 ~ 2h;
By the formaldehyde exhaust-gas running water spray-absorption in tail gas absorber produced in said process, the formalin obtained after absorption first determines the mass fraction of wherein formaldehyde, when formaldehyde mass fraction is 1 ~ 6% in the formalin obtained, formaldehyde absorbent can be joined in hydrolysing step and use as raw material;
(4) neutralize: the NaOH solution adding mass fraction 16 ~ 25% in reactor B, control temperature is at 60 ~ 75 DEG C, when in and still in material pH value reach 7 ~ 8 time, stop adding NaOH solution, can obtain solid content be 30 ~ 50% mass percents take carbolineum as the anthracene system sulfonate additive finished product of primary raw material.
In step (2), cooling refers to that in reacting kettle jacketing, pass into cold conduction oil lowers the temperature.
Production technology of the present invention compared with prior art, has the following advantages: 1, non-exhaust emission in production process, environmental friendliness.2, the waste liquid absorbing tail gas is reused for the production of additive, turns waste into wealth.The beneficial effect of production technology of the present invention is to recycle waste resource, solves by producing the environmental pollution brought simultaneously.Through probationary certificate, the Additive Properties that the present invention produces without discharge technology still can meet the means of transportation such as pumping, atomization and combustion requirements, is applicable to the coal sample of different regions.
Accompanying drawing explanation
Accompanying drawing 1 is the process chart of invention.
Detailed description of the invention
The present invention is the pipeline setting up concentration of formaldehyde on-line water flushing instrument, naoh concentration on-line water flushing instrument and the reuse of tail gas absorption liquid in traditional handicraft device.In production process, the form waste gas of sulfur dioxide of generation is absorbed via the dilute solution of sodium hydroxide that mass fraction is 8 ~ 10%, adopt the online concentration meter of NaOH to measure naoh concentration in absorbing liquid, the absorbing liquid reaching concentration index scope (1% ~ 5%) be directly used in configuration and workshop section 20% alkali lye.Absorbed via running water by the formaldehyde exhaust-gas of generation in production process, adopt formaldehyde concentration detection instrument to measure concentration of formaldehyde in absorbing liquid, the absorbing liquid reaching concentration index scope (1% ~ 6%) is directly used in the hydrolysis water of hydrolysis workshop section.
Embodiment 1:
The anthracene system sulfonate additive that it is primary raw material that the present embodiment relates to carbolineum (concrete employing one carbolineum), concrete technology condition is as follows:
(1) sulfonation: under normal temperature, the carbolineum 2300kg measured is added in reactor A and be preheated to 110 DEG C, by flowmeter, 98% quantitative concentrated sulfuric acid 2000kg is added in reactor A, drip process control at 0.5h, afterwards the temperature of reactor A is risen to 125 DEG C, insulation reaction 1.5h.
It is sodium hydroxide solution spray-absorption in acid gas absorption tower of 10% by the sulfur dioxide gas mass fraction produced in course of reaction.The spent lye obtained after absorption first adopts Potassium Hydrogen Phthalate titration concentration of sodium hydroxide solution to be 5%, again spent lye is back to use and joins alkali groove, with mass fraction be 32% liquid caustic soda and running water be that the sodium hydroxide solution of 20% is for neutralization procedure according to the proportions mass mark after calculating.
(2) be hydrolyzed: sulfonation terminates rear stoppings and heating, and reacting kettle jacketing passes into cold conduction oil and is cooled to 110 DEG C, is the formalin 1.5m of 6% by the mass fraction obtained in step (3) i.e. condensation step formaldehyde tail gas absorber while cooling
3add in reactor, at 110 DEG C of hydrolysis 0.5h.
(3) condensation: deliver in reactor B by the material after hydrolysis, the mass fraction measured, at 60 DEG C, is the formalin 1100kg of 37% by still temperature control, add in reactor B through formaldehyde head tank and flowmeter, drip process control at 1h, temperature rises to 80 DEG C subsequently, insulation 1.5h.
The formaldehyde gas running water spray-absorption in formaldehyde absorbing tower produced by above-mentioned condensation step, the formalin after absorption is back to step (2) i.e. hydrolysing step after measuring concentration.
(4) neutralize: in reactor B, progressively add the mass fraction prepared in advance in step (1) is the NaOH solution of 20%, control temperature is at 70 DEG C, when in and still in material pH value reach 7.2 time, stop adding NaOH solution, the additive finished product that solid content mass percent is 41.46% can be obtained.
Prepared by water-coal-slurry:
After coal grinding, be configured to certified reference coal according to size distribution profile.The consumption of required coal sample, additive and water is calculated according to the water coal slurry concentration set and additive addition.By additive and water Homogeneous phase mixing after accurately taking, add quantitative coal dust gradually when stirring, controlling rotating speed is that namely 1200rpm homogenizing 10min makes water-coal-slurry, evaluation test water coal slurry concentration, viscosity and syneresis rate.
In hydrolysis dilution water content of formaldehyde to be 6%, 20%NaOH solution naoh concentration be 5% the preparation of acid gas absorbing liquid, obtained additive product slurry performance evaluation result is as follows:
Embodiment 2:
Blank test: not containing formaldehyde in hydrolysis dilution water, 20wt.%NaOH solution is completely with running water preparation, and obtained additive product slurry performance evaluation result is as follows:
Embodiment 3:
In hydrolysis dilution water, content of formaldehyde is that 0.5%, 20%NaOH solution running water is prepared, and obtained additive product slurry performance evaluation result is as follows:
Embodiment 4:
In hydrolysis dilution water, content of formaldehyde is that 1.0%, 20%NaOH solution running water is prepared, and obtained additive product slurry performance evaluation result is as follows:
Embodiment 5:
In hydrolysis dilution water, content of formaldehyde is that 2.0%, 20%NaOH solution running water is prepared, and obtained additive product slurry performance evaluation result is as follows:
Embodiment 6:
In hydrolysis dilution water, content of formaldehyde is that 3.0%, 20%NaOH solution running water is prepared, and obtained additive product slurry performance evaluation result is as follows:
Embodiment 7:
In hydrolysis dilution water, content of formaldehyde is that 4.0%, 20%NaOH solution running water is prepared, and obtained additive product slurry performance evaluation result is as follows:
Embodiment 8:
In hydrolysis dilution water, content of formaldehyde is that 5.0%, 20%NaOH solution running water is prepared, and obtained additive product slurry performance evaluation result is as follows:
Embodiment 9:
In hydrolysis dilution water, content of formaldehyde is that 6.0%, 20%NaOH solution running water is prepared, and obtained additive product slurry performance evaluation result is as follows:
Embodiment 10:
In hydrolysis dilution water content of formaldehyde to be 0%, 20%NaOH solution naoh concentration be 1% the preparation of acid gas absorbing liquid, obtained additive product slurry performance evaluation result is as follows:
Embodiment 11:
In hydrolysis dilution water content of formaldehyde to be 0%, 20%NaOH solution naoh concentration be 2% the preparation of acid gas absorbing liquid, obtained additive product slurry performance evaluation result is as follows:
Embodiment 12:
In hydrolysis dilution water content of formaldehyde to be 0%, 20%NaOH solution naoh concentration be 3% the preparation of acid gas absorbing liquid, obtained additive product slurry performance evaluation result is as follows:
Embodiment 13:
In hydrolysis dilution water content of formaldehyde to be 0%, 20%NaOH solution naoh concentration be 4% the preparation of acid gas absorbing liquid, obtained additive product slurry performance evaluation result is as follows:
Embodiment 14:
In hydrolysis dilution water content of formaldehyde to be 0%, 20%NaOH solution naoh concentration be 5% the preparation of acid gas absorbing liquid, obtained additive product slurry performance evaluation result is as follows:
Embodiment 15:
In hydrolysis dilution water content of formaldehyde to be 1%, 20%NaOH solution naoh concentration be 5% the preparation of acid gas absorbing liquid, obtained additive product slurry performance evaluation result is as follows:
Embodiment 16:
In hydrolysis dilution water content of formaldehyde to be 3%, 20%NaOH solution naoh concentration be 5% the preparation of acid gas absorbing liquid, obtained additive product slurry performance evaluation result is as follows:
Embodiment 17:
In hydrolysis dilution water content of formaldehyde to be 6%, 20%NaOH solution naoh concentration be 5% the preparation of acid gas absorbing liquid, obtained additive product slurry performance evaluation result is as follows:
Above-mentioned 17 example explanations, hydrolysis dilution water adopt concentration of formaldehyde lower than 6% absorption waste liquid, in and workshop section alkali lye adopt naoh concentration lower than 5% acid gas absorbing liquid be raw material produce additive, its slurry performance still can meet industrial application requirement, properties of product are suitable with the properties of product adopting running water and soda ash liquid to produce, and can realize suitability for industrialized production.
Claims (2)
1. a nothing discharge production technology for Sulfonates additive, is characterized in that, comprise the steps:
(1) sulfonation: sulfonating reaction raw material is carbolineum and mass fraction is the concentrated sulfuric acid of 98%, the two mass ratio is 1:0.6 ~ 0.9, first carbolineum is added in reactor A and be preheated to 100 ~ 120 DEG C, then by flowmeter, the concentrated sulfuric acid is dropped in reactor A, control rate of addition is 60 ~ 70kg/min, afterwards the temperature of reactor A is risen to 120 ~ 140 DEG C, insulation reaction 1 ~ 3h;
By the SO produced in said process
2waste gas mass fraction is sodium hydroxide solution spray-absorption in acid gas absorption tower of 8 ~ 10%, the spent lye obtained after absorption first determines the concentration of wherein NaOH, again this spent lye is back to use the sodium hydroxide solution that the liquid caustic soda of liquid caustic soda or the mass fraction 32% of joining alkali groove and mass fraction 32% and water are mixed with mass fraction 16 ~ 25%, then this sodium hydroxide solution is joined in neutralization procedure uses as raw material;
(2) be hydrolyzed: sulfonation procedure terminates rear stopping heating, be cooled to 100 ~ 120 DEG C, while cooling by mass fraction be 1 ~ 6% formaldehyde absorbent add in reactor, total quality of material ratio that this formaldehyde absorbent and step (1) obtain is 1:1.5 ~ 2, at 100 ~ 120 DEG C of hydrolysis 0.5 ~ 1.5h;
(3) condensation: the material after hydrolysis is delivered in reactor B, still temperature control is at 50 ~ 70 DEG C, the formalin of mass fraction 36.7% ~ 37.4% is added dropwise in reactor B, total quality of material that this formalin and step (2) obtain is than being 1:6 ~ 7, rate of addition is 10 ~ 16kg/min, temperature rises to 80 ~ 90 DEG C subsequently, insulation 1 ~ 2h;
By the formaldehyde exhaust-gas running water spray-absorption in tail gas absorber produced in said process, the formalin obtained after absorption first determines the mass fraction of wherein formaldehyde, when formaldehyde mass fraction is 1 ~ 6% in the formalin obtained, formaldehyde absorbent can be joined in hydrolysing step and use as raw material;
(4) neutralize: the NaOH solution adding mass fraction 16 ~ 25% in reactor B, control temperature is at 60 ~ 75 DEG C, when in and still in material pH value reach 7 ~ 8 time, stop adding NaOH solution, can obtain solid content be 30 ~ 50% mass percents take carbolineum as the anthracene system sulfonate additive finished product of primary raw material.
2. the nothing discharge production technology of a kind of Sulfonates additive as claimed in claim 1, is characterized in that: in step (2), cooling refers to that in reacting kettle jacketing, pass into cold conduction oil lowers the temperature.
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| CN104633674A (en) * | 2015-01-30 | 2015-05-20 | 宜兴市兴合树脂有限公司 | Incinerator waste heat absorption device |
| CN106854167B (en) * | 2015-12-08 | 2019-03-12 | 中国石油天然气股份有限公司 | A method of producing petroleum sulfonate |
| CN105695001A (en) * | 2016-02-17 | 2016-06-22 | 兖矿水煤浆气化及煤化工国家工程研究中心有限公司 | Tar-type coal water slurry additive prepared from composite raw materials and production technology of tar-type coal water slurry additive |
| CN114288829B (en) * | 2021-12-29 | 2023-03-17 | 赞宇科技集团股份有限公司 | Comprehensive recovery device and recovery process for AES tail gas absorption liquid |
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| CN101333469A (en) * | 2008-01-22 | 2008-12-31 | 南京信息工程大学 | Synthesizing and using method of coal water slurry additive agent |
| CN101497506A (en) * | 2009-03-20 | 2009-08-05 | 武汉市联合石油化工有限责任公司 | Process for preparing modified naphthalene series water reducing agent |
| CN101797471A (en) * | 2010-04-16 | 2010-08-11 | 惠州市红墙化学建材有限公司 | Treating and recycling method of tail gas generating in sulfonated naphthaldehyde water reducing agent production and special equipment |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101333469A (en) * | 2008-01-22 | 2008-12-31 | 南京信息工程大学 | Synthesizing and using method of coal water slurry additive agent |
| CN101497506A (en) * | 2009-03-20 | 2009-08-05 | 武汉市联合石油化工有限责任公司 | Process for preparing modified naphthalene series water reducing agent |
| CN101797471A (en) * | 2010-04-16 | 2010-08-11 | 惠州市红墙化学建材有限公司 | Treating and recycling method of tail gas generating in sulfonated naphthaldehyde water reducing agent production and special equipment |
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