CN108946697A - A kind of processing method using waste sulfuric acid from alkylation production biomass carbon - Google Patents

A kind of processing method using waste sulfuric acid from alkylation production biomass carbon Download PDF

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Publication number
CN108946697A
CN108946697A CN201810872200.4A CN201810872200A CN108946697A CN 108946697 A CN108946697 A CN 108946697A CN 201810872200 A CN201810872200 A CN 201810872200A CN 108946697 A CN108946697 A CN 108946697A
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sulfuric acid
biomass
acid
biomass carbon
waste sulfuric
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周志茂
王慧
刘瑞霞
李世飞
崔改静
张锁江
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Institute of Process Engineering of CAS
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Institute of Process Engineering of CAS
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00Carbon; Compounds thereof
    • C01B32/05Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30

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  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Processing Of Solid Wastes (AREA)

Abstract

The invention discloses a kind of processing methods using alkylation spent acid production biomass carbon, belong to field of environment engineering.Biomass is added in alkylation spent acid by the present invention using biomass as raw material, and heating makes the polymerization charing under effect of sulfuric acid of the molten oil of the acid in biomass and Waste Sulfuric Acid obtain biomass carbon.The biomass carbon yield that this method obtains is greater than 60%, and no dioxin significantly reduces charcoal discharge, reduces energy consumption, realize the inexpensive charing process of biomass, meets Green Chemistry requirement.

Description

A kind of processing method using waste sulfuric acid from alkylation production biomass carbon
Technical field
The present invention relates to a kind of processing methods using waste sulfuric acid from alkylation production biomass carbon, belong to environmental project neck Domain.
Technical background:
Waste Sulfuric Acid results from the production process of the fine chemical products such as nitrification, sulfonation, alkylation, the esterification of organic matter, Mineral products processing, petroleum refining, national defense industry etc. are arisen in, the Waste Sulfuric Acid generated in production process is always to perplex manufacturing enterprise A great problem.Country's sulfuric acid process alkylation production capacity is more than 15,000,000 tons at present, such as will have 1,500,000 tons or more of sulfur waste up to production Acid.The molten oil of acid rouge, acid and water account for about 10-15% or so in waste sulfuric acid from alkylation, and appearance is brown or dark brown and has strong Strong penetrating odor.It is domestic big if executed in strict accordance with the environmental protection policy and regulation on Management of Drug-Making Chemicals of country The enterprise that majority generates Waste Sulfuric Acid will shut down.Since Waste Sulfuric Acid is a kind of liquid, row steals and puts to come than solid waste and exhaust gas steathily It is convenient and hidden, it therefore, is said from the angle of environmental protection, the improvement of Waste Sulfuric Acid is just extremely urgent.
The molten oil of acid in waste sulfuric acid from alkylation becomes the difficult point that sulfuric acid is administered, and industry at present is commonly high temperature pyrolytic cracking (HTP), The organic matters such as the molten oil of the acid generation carbon dioxide that burn at high temperature is discharged into atmosphere, and other methods are difficult to promote due to economy Using.Increasingly strict with environmental requirement, low cost, the processing of recycling sulfuric acid alkylation spent acid are imperative.It is Chinese special Sharp CN201610682877.2 and CN201710946286.5 propose the molten oil of acid in alkylation spent acid be height it is unsaturated and from The complex mixture of sonization, using the unsaturated double-bond and hydrogen bond of these molten hydrocarbon molecules of acid, intensified acid is molten in strong acidic environment The reaction such as esterification, sulfonation, polymerization, charing of oil, is allowed to generate the charcoal base acid material containing groups such as sulfuryl, sulfonic groups, and Realize the separation of acid molten oil and sulfuric acid.Thus environmental pollution can not only be mitigated significantly by carrying out resource utilization to Waste Sulfuric Acid, but also can be returned A part of sulfuric acid resource and carbon resource are received, lower reaction temperature significantly reduces recycling energy consumption, has great economy Benefit and environmental benefit.
Biomass carbon (Biochar), also referred to as charcoal, biological carbon, biomass carbon, biomass char etc..As a kind of soil Earth modifying agent, charcoal forms the soil carbon combination of an indomitable carbon negativity, and carbon dioxide storage in atmosphere is arrived In the carbon base in soil of highly resistant.After applied charcoal in soil, the enhancing of nutrition persistence not only reduces crop to fertilizer The demand of material, and the influence certain for weather and environment.
The raw material sources of charcoal are very extensive, according to the literature, many agriculture and forestry by-products, for example, jujube core, walnut shell, Walnut shell, useless tealeaves, corncob, cocoanut shell, beet root, peanut shell, rice hulls, levant cotton exocarp, banana skin, bamboo waste, dento liva, Cherry stone, orange peel, coffee beanpod, corn stover and cassava skin etc. are tried the charcoal for being used to prepare low cost.Due to For carbon atom to each other with the combination of extremely strong affinity, charcoal has very high chemistry and biology stability, and soluble pole It is low.These fundamental propertys of charcoal make it have absorption property, catalytic performance and antibiont capacity of decomposition, agricultural, the energy, The fields such as environment are all widely used.
The influence of biomass carbon includes improving soil texture, improves aggregate stability, improves soil water capacity, is promoted micro- Biological growth, and finally improve the productivity (10%) of soil.While improving crop yield, biomass carbon can also be quick Soil organic carbon is improved, N2O discharge amount and Heavy Metals in Soil Contaminated biological effectiveness are reduced.Soil improvement and upgrading are imitated It answers, especially carbon fixation and emission reduction is still current protrusion demand.Waste charing has not only handled the wastes such as stalk, avoids The directly discharge of burning or heap buried decomposition, increases soil organism carbon storehouse, also significantly improves the physical property of soil, promotees It into biological growth and activity, improves fertility and reduces risk of environmental pollution, be the important channel of soil sustainable management. The agricultural wastes such as stalk are not utilized effectively, and a large amount of directly burn exacerbates atmosphere pollution.In national green development strategy Under frame, the outlet of the sustainable management of soil and changing rejected material to useful resource circulation as complementary agricultural sustainable development.
Preparing the most common method of charcoal is pyrolysis method, i.e., thermally decomposes in no oxygen or oxygen-limited condition environment Organic material, the solid matter of formation, main component are carbon, hydrogen, oxygen, nitrogen etc., also include a small amount of microelement, carbon containing Amount is generally 60% or more.In carbonization process, non-carbon element is decomposed and evolution forms hole configurations, therefore has certain hole Porosity and specific surface area.Charcoal surface functional group very abundant includes a variety of groups such as carboxyl, phenolic hydroxyl group, acid anhydrides.Pyrolysismethod Handle biomass adaptability it is relatively preferable, in terms of process performance index also have some superiority, decrement than reach 95% with On, and auxiliary fuel, recoverable energy are not needed in operation, waste is not required to classify and pre-process.But waste gas from incinerator processing dress It is serious to set acidification, dioxin cannot be guaranteed that stably reaching standard discharges, and overhaul costly.And the control for dioxin, it is biomass Burn problem the most intractable.Since dioxin generting machanism is considerably complicated, according to domestic literature, it is known that constructive ways conclude 2 A aspect: 1) predecessor heterogeneous catalytic reaction forms dioxin.That is the organic compounds such as polystream, chlorophenols, PVC, in metal At catalyst (copper chloride, iron chloride etc.) and 450~700 DEG C, reacts and generate dioxin;2) it recombines reaction and forms two English is disliked, i.e., (coke flies for imperfect combustion particulate organic carbon (propylene, toluene, chlorobenzene etc.) and giant molecule carbon structure in flying dust Ash, residual carbon etc.) at 250~850 DEG C, by different catalyst, aoxidized, chlorination, polymerization form dioxin.So The optimum synthesising temperature of dioxin is 250~400 DEG C.
Sulfuric acid charring is at a lower temperature to be taken off carbon containing biomass material using the dehydration property and highly acid of the concentrated sulfuric acid Water charing, obtains the process of biomass carbon material.CN103157509, CN103157512 disclose the concentrated sulfuric acid and bagasse (or Rice husk) Hybrid Heating is partially carbonized prepares solid sulfoacid, and CN100421793, CN100421792 are disclosed with plant material or carbon The method that hydrate prepares solid sulfoacid, but be carbonized not exclusively, solid carbon yield is low, and Organic Materials of Spent acid content is high.Once There are research sulfuric acid catalysis charing sludge and cotton, but degree of carbonization is low, the carbide granularity for needing to carbonize and generate twice It is small, it is soluble in sulfuric acid, is difficult to separate, wash high organic content in acid, can not comprehensively utilize.Therefore, develop it is a kind of it is low at Originally, the recycling processing method of innoxious biomass, has great importance.
Summary of the invention
For the technical problems in the prior art, the present invention provides a kind of waste sulfuric acid from alkylation to produce biomass carbon The processing method of change.
The molten hydrocarbon of acid contained in waste sulfuric acid from alkylation is the complex mixture that height is unsaturated and ionizes, biomass material Short texture, distribution dispersion, occupied space are big.A large amount of foam can be generated in waste sulfuric acid from alkylation heating polymerization process, and is given birth to The molecule of these easy bubbles just can be absorbed in the loose structure of substance, improves the carbonization degree of the molten oil of acid in alkylation spent acid. Using the unsaturated double-bond and hydrogen bond of these molten hydrocarbon molecules of acid, by the effect of sulfuric acid, biomass is in strong acidic environment neutralizing acid The reactions such as the raw polymerization of molten fry dried food ingredients, charing are carbonized completely, are reacted the organic matter in biomass and spent acid and are generated resourcebility benefit Biomass carbon.
The present invention realizes the resource utilization benefit of organic matter in biomass and waste sulfuric acid from alkylation using biomass as raw material With reducing carbon emission, obtained biomass carbon and diluted acid have biggish application value.The processing method reaction step is few, Energy consumption is low, realizes the charing process of low-cost bio matter, applied widely, meets Green Chemistry requirement.Biomass Carbonizing treatment method includes the following steps that be heated to biomass after (1) mixes biomass with waste sulfuric acid from alkylation carbonizes completely, Obtain mixture;(2) mixture that step (1) generates is down to room temperature, solvent is added into mixture, stirring is adsorbed into charcoal Acid all dissolve out, washing, drying obtain biomass carbon and diluted acid.
The weight ratio of waste sulfuric acid from alkylation and biomass is 0.1~10:1.
The temperature of heating reaction is 100~300 DEG C in step (1), and the time is 0.5~4 hour.
Solvent is water, dilute sulfuric acid, phosphoric acid,diluted or ammonium hydroxide, sig water in step (2);The additional amount of solvent is sulfuric acid weight 1~10 times, preferably 1~5 times.Dilute sulfuric acid, phosphoric acid,diluted refer to mass percentage in 30% acid below.
Available dilute sulfuric acid or sulfate and biomass carbon after washing, biomass carbon and with sulfate compositions be biology Matter charcoal fertilizer, or as the raw material of biomass carbon fertilizer.
The temperature dried in step (2) is 60~200 DEG C;The pressure of drying is -0.1~0.1MPa;The time of drying is 0.5~4 hour;The number of washing is 1~6 time.
The present invention realizes the resource utilization of organic matter and acid in biomass and waste sulfuric acid from alkylation using biomass as raw material It utilizes, reduces carbon emission, obtained biomass carbon and diluted acid have biggish application value;Reduce reaction step, reduce Energy consumption, Biomass are biomass carbon, high conversion rate.Due to being provided to biomass and the organic Waste Sulfuric Acid of high concentration Sourceization utilizes can not only mitigate environmental pollution significantly, but also a part of sulfuric acid resource and carbon resource can be recycled, and lower reaction temperature It significantly reduces recycling energy consumption, without dioxin in discharge gas, there is great economic benefit and environmental benefit.The present invention The method route of offer is short, easy to operate, low energy consumption, applied widely, meets Green Chemistry requirement.
The beneficial effects of the present invention are:
In the present invention, it is heated after biomass mixed alkyl Waste Sulfuric Acid, the molten fry dried food ingredients of acid in biomass and Waste Sulfuric Acid is raw The reactions such as polymerization, charing generate biomass carbon, improve the carbonization yield of the molten oil of acid, without dioxin in discharge gas, at reduction Content of organics in diluted acid after reason.Product is washed by solution after reaction realizes that Carbon Materials are separated with acid, respectively obtains biomass carbon And diluted acid, it can be using synthesis materials such as chemical fertilizer, bodied ferric sulfates.Biomass carbonated obtained biomass carbon has raw material sources Abundant, cheap, large specific surface area, pore structure prosperity, thermal stability and good chemical stability, can answer extensively For various fields such as agricultural, environment remediation, chemical industry, energy storages, as biomass carbon fertilizer and soil conditioner, useless underwater gold Category or the adsorbent of organic matter, the adsorbent of atmosphere pollution, acid catalyst or catalyst carrier, electrode and super capacitor material Deng having broad application prospects.
Specific embodiment
The technical scheme of the invention is further explained by means of specific implementation.Those skilled in the art should be bright , the described embodiments are merely helpful in understanding the present invention, should not be regarded as a specific limitation of the invention.
Embodiment 1
Weigh waste sulfuric acid from alkylation 102.5g (acid concentration 89.2% contains organic matter 6.8%) in a round bottom flask (250mL) is added the rice husk of spent acid quality 20%, is increased to 160 DEG C from room temperature, then maintains 3.5h, be cooled to room temperature, weigh The water that 1 times of spent acid quality is added in round-bottomed flask, stirs 30min, and water re-using washing, stirring 3 times obtain filtrate (dilute sulphur Acid solution) and filter cake (biomass carbon), filtrate is collected into beaker, and the COD value of filtrates tested is 469.7mg/L, in stirring Under the conditions of be slowly added into ammonium hydroxide (25~28wt%) until solution is in neutrality, then evaporate solution to there is ammonia sulfate crystal precipitation. Filter cake is washed with deionized until neutrality, dries 2 hours at 100 DEG C, 0.1MPa, obtain biomass carbon 21.96g.
Embodiment 2
Weigh waste sulfuric acid from alkylation 103.4g (acid concentration 89.2% contains organic matter 6.8%) in a round bottom flask (250mL) is added the sawdust of spent acid quality 40%, is increased to 220 DEG C from room temperature, then maintains 3h, be cooled to room temperature, weigh useless The water of 1 times of sour quality is added in round-bottomed flask, stirs 30min, and water re-using washing, stirring 3 times obtain filtrate (dilute sulfuric acid Solution) and filter cake (Carbon Materials), filtrate is collected into beaker, and the COD value of filtrates tested is 361.7mg/L, in the condition of stirring Under be slowly added into ammonium hydroxide (25~28wt%) until solution is in neutrality, then evaporate solution to there is crystal precipitation.Use deionized water Filter cake is washed until neutrality, dries 3 hours at 150 DEG C, 0.05MPa, obtain biomass carbon 38.72g.
Embodiment 3
Weigh waste sulfuric acid from alkylation 102.9g (acid concentration 89.2% contains organic matter 6.8%) in a round bottom flask (250mL) is added 1 times of spent acid quality of rice husk, is increased to 220 DEG C from room temperature, then maintains 2h, be cooled to room temperature, weigh sulphur The water of 1 times of sour quality is added in round-bottomed flask, stirs 30min, and water re-using washing, stirring 3 times obtain filtrate (dilute sulfuric acid Solution) and filter cake (Carbon Materials), filtrate is collected into beaker, the COD value 634.9mg/L of filtrates tested, under stirring conditions Ammonium hydroxide (25~28wt%) is slowly added into until solution is in neutrality, then evaporates solution to there is crystal precipitation.It is washed with deionized water Filter cake is washed until neutrality, dries 3 hours at 200 DEG C, 0.01MPa, obtain biomass carbon 87.9g.
Embodiment 4
Weigh waste sulfuric acid from alkylation 101.5g (acid concentration 89.2% contains organic matter 6.8%) in a round bottom flask (250mL) is added the corn stover of spent acid quality 10%, is increased to 240 DEG C from room temperature, then maintains 1h, be cooled to room temperature, claim The water for taking spent acid quality equal is added in round-bottomed flask, stirs 30min, and it is (dilute to obtain filtrate for water re-using washing, stirring 3 times Sulfuric acid solution) and filter cake (Carbon Materials), filtrate is collected into beaker, the COD value 867.9mg/L of filtrates tested.Use deionized water Filter cake is washed until neutrality, dries 4 hours at 100 DEG C, 0.1MPa, obtain biomass carbon 12.5g.
Embodiment 5
Weigh waste sulfuric acid from alkylation 103.8g (acid concentration 89.2% contains organic matter 6.8%) in a round bottom flask (250mL) is added the wheat stalk of spent acid quality 10%, is increased to 160 DEG C from room temperature, then maintains 3.5h, be cooled to room temperature, The water for weighing spent acid quality 150% is added in round-bottomed flask, stirs 30min, is washed repeatedly 2 times, obtaining filtrate, (dilute sulfuric acid is molten Liquid) and filter cake (Carbon Materials), filtrate is collected into beaker, the COD value 1591.4mg/L of filtrates tested.Filter is washed with deionized Cake dries 2 hours at 100 DEG C, 0.1MPa until neutrality, obtains biomass carbon 12.5g.
Comparative example
It weighs sulfuric acid 102.7g (250mL) in a round bottom flask, the rice husk of sulfuric acid quality 50% is added, is increased to from room temperature 200 DEG C, 3.5h is then maintained, is cooled to room temperature, 1 times of sulfuric acid quality of water is weighed and is added in round-bottomed flask, stirs 30min, Water re-using washing, stirring 3 times, obtain filtrate (dilution heat of sulfuric acid) and filter cake (Carbon Materials), collect filtrate into beaker, test The COD value 3524.8mg/L of filtrate.Filter cake is washed with deionized until neutrality, dries 2 hours at 100 DEG C, 0.1MPa, obtain To biomass carbon 32.9g.
As it can be seen that waste sulfuric acid from alkylation and biomass Co-carbonization reaction efficiency ratio using bright sulfur acid with it is biomass carbonated high, Reaction process is mild, biomass carbon high income, and content of organics is few in dilution heat of sulfuric acid.
The Applicant declares that a kind of charing process side of the present invention is explained by the above embodiments biomass of the invention Method, but the invention is not limited to above-mentioned processing steps, that is, it is real not mean that the present invention must rely on above-mentioned processing step ability It applies.It should be clear to those skilled in the art, any improvement in the present invention, to the equivalent of raw material selected by the present invention Replacement and addition, the selection of concrete mode of auxiliary element etc., all of which fall within the scope of protection and disclosure of the present invention.

Claims (6)

1. a kind of processing method using waste sulfuric acid from alkylation production biomass carbon, it is characterised in that: biomass is added to alkane In base spent acid, it is heated to the molten oily polymerization charing under effect of sulfuric acid of acid that 100~300 DEG C make in biomass and Waste Sulfuric Acid and obtains Biomass carbon.The following steps are included:
(1) biomass is dry, crush as powdered biomass;
(2) it is heated to 100~300 DEG C after mixing with waste sulfuric acid from alkylation to carbonize biomass completely, obtains mixture;
(3) mixture that step (2) generate is down to room temperature, solvent is added into mixture, it is complete to stir the acid adsorbed into charcoal Portion dissolve out, washing, drying obtain biomass carbon and diluted acid.
2. a kind of processing method using waste sulfuric acid from alkylation production biomass carbon according to claim 1, feature exist In: the weight ratio of sulfuric acid described in step (2) and biomass is 0.1~10:1.
3. a kind of processing method using waste sulfuric acid from alkylation production biomass carbon according to claim 1, feature exist In: the temperature that reaction is heated described in step (1) is 160~250 DEG C, and the time is 0.5~4 hour.
4. a kind of processing method using waste sulfuric acid from alkylation production biomass carbon according to claim 1, feature exist In: solvent described in step (2) is water, the dilute sulfuric acid of concentration 1%~50%, the phosphoric acid,diluted of concentration 1%~30% or concentration 1% ~30% ammonium hydroxide;The additional amount of solvent is 1~10 times of sulfuric acid weight.
5. a kind of processing method using waste sulfuric acid from alkylation production biomass carbon according to claim 1, feature exist In: the additional amount of solvent is 1~5 times of sulfuric acid weight.
6. a kind of processing method using waste sulfuric acid from alkylation production biomass carbon according to claim 1, feature exist In: the temperature dried in step (2) is 60~200 DEG C;The pressure of drying is -0.1~0.1MPa;The time of drying is 0.5~4 Hour;The number of washing is 1~6 time.
CN201810872200.4A 2018-08-02 2018-08-02 A kind of processing method using waste sulfuric acid from alkylation production biomass carbon Pending CN108946697A (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110550610A (en) * 2019-10-18 2019-12-10 斯瑞尔环境科技股份有限公司 Regeneration treatment method of alkylation waste sulfuric acid
CN111333905A (en) * 2020-04-20 2020-06-26 中国科学院过程工程研究所 Recovery method of fiber reinforced composite material
CN111533584A (en) * 2020-06-12 2020-08-14 山东鲁北化工股份有限公司 Preparation method of biomass sulfonated carbon based diammonium phosphate
CN111646856A (en) * 2020-06-12 2020-09-11 山东鲁北化工股份有限公司 Preparation method of biomass sulfonated carbon-based compound fertilizer
CN112897503A (en) * 2021-01-25 2021-06-04 上海应用技术大学 Acid modification preparation method of biomass charcoal material with toluene adsorption effect
CN113415803A (en) * 2021-08-12 2021-09-21 中国科学院生态环境研究中心 Waste treatment method

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Publication number Priority date Publication date Assignee Title
CN105000558A (en) * 2015-08-14 2015-10-28 赵常然 Method for directly preparing activated carbon in waste acid
CN105858622A (en) * 2016-05-19 2016-08-17 广西南宁东和新赢环保技术有限公司 Alkylation waste sulfuric acid resource recycling method

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105000558A (en) * 2015-08-14 2015-10-28 赵常然 Method for directly preparing activated carbon in waste acid
CN105858622A (en) * 2016-05-19 2016-08-17 广西南宁东和新赢环保技术有限公司 Alkylation waste sulfuric acid resource recycling method

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110550610A (en) * 2019-10-18 2019-12-10 斯瑞尔环境科技股份有限公司 Regeneration treatment method of alkylation waste sulfuric acid
CN111333905A (en) * 2020-04-20 2020-06-26 中国科学院过程工程研究所 Recovery method of fiber reinforced composite material
CN111533584A (en) * 2020-06-12 2020-08-14 山东鲁北化工股份有限公司 Preparation method of biomass sulfonated carbon based diammonium phosphate
CN111646856A (en) * 2020-06-12 2020-09-11 山东鲁北化工股份有限公司 Preparation method of biomass sulfonated carbon-based compound fertilizer
CN112897503A (en) * 2021-01-25 2021-06-04 上海应用技术大学 Acid modification preparation method of biomass charcoal material with toluene adsorption effect
CN113415803A (en) * 2021-08-12 2021-09-21 中国科学院生态环境研究中心 Waste treatment method

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