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CN102911690A - Method for preparing fuel oil from waste paper waste residue - Google Patents

Method for preparing fuel oil from waste paper waste residue Download PDF

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Publication number
CN102911690A
CN102911690A CN201210336113XA CN201210336113A CN102911690A CN 102911690 A CN102911690 A CN 102911690A CN 201210336113X A CN201210336113X A CN 201210336113XA CN 201210336113 A CN201210336113 A CN 201210336113A CN 102911690 A CN102911690 A CN 102911690A
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waste
waste paper
fuel oil
bamboo charcoal
reaction
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CN102911690B (en
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裴文
孙莉
戚新军
胡卫雅
赵婷
单东方
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Guangdong Gaohang Intellectual Property Operation Co ltd
Zhongrong Technology Corp ltd
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Zhejiang University of Technology ZJUT
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Abstract

本发明公开了一种利用废纸废渣制备燃料油的方法：将利用废纸造纸后产生的废渣进行预处理，取预处理后的废纸废渣为原料，以竹炭磺化固体酸为催化剂，在100~500℃下裂解反应0.5~10h，反应结束后，将裂解液进行蒸馏处理，收集40~330℃的馏分作为燃料油；本发明所述利用固体酸催化剂生产燃料油的方法无固废生成，环境友好，且本发明方法适合于一定规模的工业化生产，是一条变废为宝的绿色清洁生产技术，目前尚未有工业化生产的应用报道。The invention discloses a method for preparing fuel oil by using waste paper residues: pretreating the waste residues produced after making paper using waste paper, taking the pretreated waste paper residues as raw materials, using bamboo charcoal sulfonated solid acid as a catalyst, and using bamboo charcoal as a catalyst. Cracking reaction at 100-500°C for 0.5-10h, after the reaction is over, distill the lysate, and collect the fraction at 40-330°C as fuel oil; the method for producing fuel oil using a solid acid catalyst in the present invention does not generate solid waste , environment-friendly, and the method of the present invention is suitable for a certain scale of industrial production, is a green and clean production technology that turns waste into wealth, and there is no application report for industrial production at present.

Description

A kind of method of utilizing the waste paper waste residue to prepare oil fuel
(1) technical field
The present invention relates to a kind of waste paper waste residue utilization technology, especially a kind ofly use novel carbon back sulfonic acid type solid acid as catalyzer, utilize cracking technique to carry out the green process technology of waste paper waste residue liquefaction.
(2) background technology
The waste paper recycling is an effective way that solves papermaking shortage of raw materials problem, can saving resource, reduce cost, and be the important measures that China's paper industry solves the fibrous material difficulty.But, to produce a large amount of waste residues after utilizing regenerated papermaking.The waste paper waste residue that produces every day at present by statistics has more than the upper kiloton.The main component of waste residue is plastic waste by analysis, because plastic refuse is not perishable, has had a strong impact on the ecotope of the earth.Therefore, the improvement of plastic waste is very urgent.
Carbon back sulfonic acid type solid acid is a kind of solid acid catalyst of in recent years people's research and development, is to utilize biomass control charing to be prepared into solid sulfoacid, has caused in recent years people's great attention.Utilize solid acid as heterogeneous catalyst, generally have not etching apparatus, pollution is little, high temperature resistant, aftertreatment is simple, easily separated and low cost and other advantages, and obtained broad research and application in the acid catalysis field.Therefore, new and effective solid acid catalyst is used for the waste paper waste residue---the made from used plastics oil tech has great significance, and there is not yet report in the application aspect the waste paper waste residue catalytic pyrolysis.
(3) summary of the invention
The object of the invention provides a kind of novel carbon back sulfonic acid type solid acid catalyst that utilizes, and adopts cracking, distillation technique to realize waste sludge from paper mill catalyse pyrolysis liquefaction technology.
The technical solution used in the present invention is:
A kind of method of utilizing the waste paper waste residue to prepare oil fuel, described method is: will utilize the waste residue that produces behind the regenerated papermaking to dry comminution pretreatment, getting pretreated waste paper waste residue is raw material, take bamboo charcoal sulfonation solid acid as catalyzer, at 100 ~ 500 ℃ of lower scission reaction 0.5 ~ 10h, after reaction finishes, lysate is distilled processing, collect 40 ~ 330 ℃ the cut oil that acts as a fuel.Described bamboo charcoal sulfonation solid acid is that catalyzer is take the bamboo bits as raw material, carries out the pyrolysis carbonization, then sulfonation in the vitriol oil or oleum, a kind of new catalyst of preparation not being higher than under 600 ℃ the condition.
Further, described oven dry comminution pretreatment is first the waste residue that produces behind the regenerated papermaking to be dried to moisture content to be lower than 5%, then pulverizes, and obtains pretreated waste paper waste residue.
Further, after described lysate distillation is processed, collect respectively 40 ~ 190 ℃ cut as gasoline, collect 250 ~ 330 ℃ cut as diesel oil.
Further, described sulfonic acid type solid acid and the pretreated waste paper waste residue mass ratio that feeds intake is 0.01 ~ 0.3:1.
Further, described reaction is at 300 ~ 400 ℃ of lower scission reaction 1 ~ 5h.
The catalyzer that adopts during catalytic cracking reaction of the present invention belongs to the solid sulfoacid class catalyzer of biomass control charing preparation, be preferably bamboo charcoal sulfonation solid acid catalyst, " preparation of sulfonation bamboo charcoal, sign and acid catalytic properties thereof " such as preparation method's reference literature Xu Qiong, new carbon, 2011,26(2), 103-108.
Catalytic cracking reaction mechanism can be explained with the carbonium ion theory.The alkene that thermo-cracking produces long carbochain occurs first in waste sludge from paper mill, and then alkene enters and obtains H on the catalyst surface +And the formation carbonium ion, carbonium ion fragments into first primary in the β position, secondary carbon ion, then is isomerizated into more stable tertiary carbon positive ion, and last, stable tertiary carbon positive ion is with H +Return catalyzer, itself becomes alkene.Isomerization can make non-straight chain hydrocarbon molecule greatly increase, and the straight chain hydrocarbon molecule reduces.
Described cleavage method is catalytic pyrolysis under heating, makes the chain rupture of polyolefine macromole, and making its cracking is small molecules.C in these small molecules 5H 12～C 11H 24Deng being exactly gasoline component; C 12H 26～C 20H 42Be diesel component.Or 40～190 ℃ be the gasoline distillation stage, and 250～330 ℃ is the diesel oil distillation stage.
Further, bamboo charcoal sulfonation solid acid catalyst of the present invention prepares as follows: (1) is with the H of dry bamboo bits in mass concentration 30～80% 3PO 4After soaking 1～20h(preferred 3 ~ 20h) in the aqueous solution, use the Büchner funnel suction filtration, get filter cake a and obtain dried filter cake at 100 ℃ of lower dry 24h, then dried filter cake is carried out pyrolysis in tube furnace, namely the speed with 30 ℃/min is warming up to 110 ℃, be incubated 3 hours, naturally cool to after the room temperature with deionized water wash to neutral, obtain bamboo charcoal after the drying; Described dry bamboo bits and H 3PO 4The mass ratio of the aqueous solution is 1:3～10; (2) bamboo charcoal is added SO 3In the oleum of massfraction 50%, be warming up to 100 ℃ and constant temperature sulfonation 2h, add deionized water cooling termination reaction, filter, get filter cake b with deionized water wash to detecting till the sulfate radical-free ion with barium chloride solution, obtain bamboo charcoal sulfonation solid acid catalyst after the drying; Described bamboo charcoal and oleum mass ratio are the preferred 1:5 of 1:1～5().
Further, the method of utilizing the waste paper waste residue to prepare oil fuel of the present invention is carried out as follows: will utilize the waste residue that produces behind the regenerated papermaking to be dried to moisture content and be lower than 5%, getting pretreated waste paper waste residue mixes with mass ratio 1:0.01 ~ 0.3 with bamboo charcoal sulfonation solid acid and is placed in the scission reaction still, at 300 ~ 400 ℃ of lower scission reaction 1 ~ 5h, after reaction finishes, filtering reaction raw materials (waste residue and bamboo charcoal sulfonation solid acid are carbonized), lysate is transferred to distills processing in the still kettle, collect respectively 40 ~ 190 ℃ cut as gasoline component, collect 250 ~ 330 ℃ cut as diesel oil.
Filter cake a of the present invention and filter cake b are filter cake, and for ease of distinguishing different step acquisition filter cake difference and naming, alphabetical a and b itself do not have implication.
The waste residue that produces after waste paper (usually waste paper on adhesive tape the impurity such as the waste or used plastics are arranged) papermaking that utilizes of the present invention mainly is: can't be produced some waste materials, the impurity that utilize, such as surplus waste or used plastics out in the waste paper pulp-making process etc.
Compared with prior art, the method of utilizing solid acid catalyst to produce oil fuel of the present invention generates without solid waste, environmental friendliness, and the inventive method is suitable for the suitability for industrialized production of certain scale, be a green clearer production technology of turning waste into wealth, the application report of suitability for industrialized production is not yet arranged at present.
(4) embodiment
The present invention is described further below in conjunction with specific embodiment, but protection scope of the present invention is not limited in this:
The preparation of catalyzer
Embodiment 1
1, carbonization process: dry bamboo bits 100 are restrained in the H of mass concentration 30% 3PO 4Soaked 20 hours in the aqueous solution 1000 grams, use the Büchner funnel suction filtration, get filter cake obtains impregnation of phosphoric acid at 100 ℃ of lower dry 24h bamboo bits, then in tube furnace, carry out pyrolysis, namely the temperature rise rate with 30 ℃/min is warming up to 110 ℃, is incubated 3 hours, naturally cools to room temperature (20 ℃), products therefrom to neutral, obtains bamboo charcoal with deionized water wash after the drying.
2, sulfonation process: get above-mentioned bamboo charcoal 2 grams, add SO 3Oleum 10 grams of massfraction 50%, be warming up to 100 ℃ of constant temperature sulfonation 2 hours, add deionized water cooling termination reaction, filter, with filter cake with deionized water wash to detecting till the sulfate radical-free ion with barium chloride solution, obtain bamboo charcoal sulfonation solid acid catalyst 2.2 grams after the drying, acid content is 2.01mmol/g.
Embodiment 2
1, carbonization process: dry bamboo bits 100 are restrained in the H of mass concentration 80% 3PO 4Soaked 3 hours in the aqueous solution 300 grams, use the Büchner funnel suction filtration, get filter cake at 100 ℃ of lower dry bamboo bits that obtained impregnation of phosphoric acid in 24 hours, then in tube furnace, carry out pyrolysis, namely the temperature rise rate with 30 ℃/min is warming up to 110 ℃, is incubated 3 hours, naturally cools to room temperature, products therefrom to neutral, obtains bamboo charcoal with deionized water wash after the drying.
2, sulfonation process: get above-mentioned bamboo charcoal 2 grams, add SO 3Oleum 10 grams of massfraction 50%, be warming up to 100 ℃ of constant temperature sulfonation 2 hours, add deionized water cooling termination reaction, filter, with filter cake with deionized water wash to detecting till the sulfate radical-free ion with barium chloride solution, obtain bamboo charcoal sulfonation solid acid catalyst 2.2 grams after the drying, acid content is 2.03mmol/g.
Embodiment 3
1, carbonization process: dry bamboo bits 100 are restrained in the H of mass concentration 50% 3PO 4Soaked 10 hours in the aqueous solution 600 grams, use the Büchner funnel suction filtration, get filter cake at 100 ℃ of lower dry bamboo bits that obtained impregnation of phosphoric acid in 24 hours, then in tube furnace, carry out pyrolysis, namely the temperature rise rate with 30 ℃/min is warming up to 110 ℃, is incubated 3 hours, naturally cools to room temperature, products therefrom to neutral, obtains bamboo charcoal with deionized water wash after the drying.
2, sulfonation process: get above-mentioned bamboo charcoal 2 grams, add SO 3Oleum 10 grams of massfraction 50%, be warming up to 100 ℃ of constant temperature sulfonation 2 hours, add deionized water cooling termination reaction, filter, get filter cake with deionized water wash to detecting till the sulfate radical-free ion with barium chloride solution, obtain bamboo charcoal sulfonation solid acid catalyst 2.2 grams after the drying, acid content is 2.0mmol/g.
Embodiment 4: utilize embodiment 1 catalyzer to carry out the waste sludge from paper mill cracking
To utilize the waste residue oven dry that produces after waste paper (adhesive tape has the waste paper of the impurity such as the plastics) papermaking to make moisture be lower than 5%, pulverize, getting raw material after the pulverizing and the bamboo charcoal sulfonation solid acid catalyst of embodiment 1 preparation mixes with mass ratio 1:0.3, add fluidized bed cracking still (conventional closed reactor gets final product), after charging is complete, 300 ℃ of cracking 1 hour, after reaction finishes, the filtering reaction raw materials, lysate is squeezed into still kettle (conventional still kettle), collect respectively 40～190 ℃ of effluent liquid as gasoline, 250～330 ℃ of cuts are as diesel oil.Going out oil recovery rate is 70%.HPLC detects, and the purity of gasoline and diesel oil all reaches 99.4%.
Embodiment 5: utilize embodiment 2 catalyzer to carry out the waste sludge from paper mill cracking
To utilize the waste residue oven dry that produces after waste paper (with the embodiment 4) papermaking to make moisture low 5%, pulverize, getting raw material after the pulverizing and the bamboo charcoal sulfonation solid acid catalyst of embodiment 2 preparations mixes with mass ratio 1:0.01, add the fluidized bed cracking still, 500 ℃ of cracking 10 hours, after reaction finishes, the filtering reaction raw materials, lysate is squeezed into still kettle, collect respectively 40～190 ℃ of cuts as gasoline, 250～330 ℃ of cuts are as diesel oil.Going out oil recovery rate is 75%.HPLC detects, and the purity of gasoline and diesel oil all reaches 99.6%.
Embodiment 6: utilize embodiment 3 catalyzer to carry out the waste sludge from paper mill cracking
To utilize the waste residue oven dry that produces after waste paper (with the embodiment 4) papermaking to make moisture low 5%, pulverize, getting raw material after the pulverizing and the bamboo charcoal sulfonation solid acid catalyst of embodiment 3 preparations mixes with mass ratio 1:0.15, add the fluidized bed cracking still, 400 ℃ of cracking 5 hours, after reaction finishes, the filtering reaction raw materials, lysate is squeezed into still kettle, collect respectively 40～190 ℃ of cuts as gasoline, 250～330 ℃ of cuts are as diesel oil.Going out oil recovery rate is 73%.HPLC detects, and the purity of gasoline and diesel oil all reaches 99.3%.

Claims (7)

1.一种利用废纸废渣制备燃料油的方法，其特征在于所述方法为：将利用废纸造纸后产生的废渣进行烘干粉碎预处理，取预处理后的废纸废渣为原料，以竹炭磺化固体酸为催化剂，在100~500℃下裂解反应0.5~10h，反应结束后，将裂解液进行蒸馏处理，收集40~330℃的馏分作为燃料油。1. A method for preparing fuel oil by utilizing waste paper residues, characterized in that the method is: the waste residues produced after papermaking of waste papers are used for drying and crushing pretreatment, and the waste paper residues after pretreatment are taken as raw materials, and Bamboo charcoal sulfonated solid acid is used as a catalyst, and the cracking reaction is carried out at 100-500°C for 0.5-10h. After the reaction, the lysate is distilled and the fraction at 40-330°C is collected as fuel oil. 2.如权利要求1所述利用废纸废渣制备燃料油的方法，其特征在于所述烘干粉碎预处理是先将废纸造纸后产生的废渣烘干至水分含量低于5%，然后进行粉碎，获得预处理后的废纸废渣。2. The method for preparing fuel oil from waste paper residues as claimed in claim 1, wherein the drying and crushing pretreatment is to first dry the waste residues produced after waste paper making to a moisture content lower than 5%, and then carry out Crushed to obtain the pretreated waste paper residue. 3.如权利要求1所述利用废纸废渣制备燃料油的方法，其特征在于所述裂解液蒸馏处理后，分别收集40~190℃的馏分作为汽油，收集250~330℃的馏分作为柴油。3. The method for preparing fuel oil from waste paper and residue as claimed in claim 1, characterized in that after the lysate is distilled, the cuts at 40-190° C. are collected as gasoline, and the cuts at 250-330° C. are collected as diesel oil. 4.如权利要求1所述利用废纸废渣制备燃料油的方法，其特征在于所述磺酸型固体酸与预处理后的废纸废渣投料质量比为0.01~0.3:1。4. The method for preparing fuel oil from waste paper and residue as claimed in claim 1, wherein the mass ratio of the sulfonic acid-type solid acid to the pretreated waste paper and residue is 0.01-0.3:1. 5.如权利要求1所述利用废纸废渣制备燃料油的方法，其特征在于所述反应在300~ 400℃下裂解反应1~5h。5. the method for utilizing waste paper waste residue to prepare fuel oil as claimed in claim 1, is characterized in that described reaction cracking reaction 1～5h at 300～400 ℃. 6.如权利要求1所述利用废纸废渣制备燃料油的方法，其特征在于所述竹炭磺化固体酸催化剂按如下方法制备：（1）将干燥竹屑在质量浓度30～80%的H3PO4水溶液中浸泡1～20h后，用布氏漏斗抽滤，取滤饼a在100℃下干燥24h得到干燥后的滤饼，然后将干燥后的滤饼在管式炉中进行热解，即以30℃/min的速率升温至110℃，保温3小时，自然降温到室温后用去离子水洗涤至中性，干燥后得到竹炭；所述干燥竹屑与H3PO4水溶液的质量比为1：3～10；（2）将竹炭加入SO3质量分数50%的发烟硫酸中，升温至100℃并恒温磺化2h，加入去离子水冷却终止反应，过滤，取滤饼b用去离子水洗涤至用氯化钡水溶液检测至无硫酸根离子为止，干燥后得到竹炭磺化固体酸催化剂；所述竹炭与发烟硫酸质量比为1：1～5。6. The method for preparing fuel oil by using waste paper waste residues as claimed in claim 1, characterized in that the bamboo charcoal sulfonated solid acid catalyst is prepared as follows: (1) dry bamboo chips in 30-80% H 3 After soaking in PO 4 aqueous solution for 1-20 hours, filter with Buchner funnel, take the filter cake a and dry it at 100°C for 24 hours to obtain the dried filter cake, and then pyrolyze the dried filter cake in a tube furnace , that is to raise the temperature to 110°C at a rate of 30°C/min, keep it warm for 3 hours, wash it with deionized water to neutrality after naturally cooling to room temperature, and obtain bamboo charcoal after drying; the mass of the dried bamboo chips and H 3 PO 4 aqueous solution The ratio is 1:3~10; (2) Add bamboo charcoal to oleum with 50% SO 3 mass fraction, raise the temperature to 100°C and sulfonate at constant temperature for 2 hours, add deionized water to cool to terminate the reaction, filter, and take the filter cake b Washing with deionized water until no sulfate ions are detected by barium chloride aqueous solution, and drying to obtain a bamboo charcoal sulfonated solid acid catalyst; the mass ratio of the bamboo charcoal to oleum is 1:1-5. 7.如权利要求1所述利用废纸废渣制备燃料油的方法，其特征在于所述方法按如下步骤进行：将利用废纸造纸后产生的废渣干燥至水分含量低于5%，取预处理后的废纸废渣与竹炭磺化固体酸以质量比1:0.01~0.3混合后置于裂解反应釜中，在300~400℃下裂解反应1~5h，反应结束后，滤除反应原料，将裂解液转移入蒸馏釜内进行蒸馏处理，分别收集40~190℃的馏分作为汽油组分，收集250~330℃的馏分作为柴油。7. The method for preparing fuel oil by using waste paper waste residues as claimed in claim 1, characterized in that the method is carried out as follows: the waste residues produced after papermaking using waste papers are dried to a moisture content lower than 5%, and the pretreatment The final waste paper waste and bamboo charcoal sulfonated solid acid are mixed in a mass ratio of 1:0.01~0.3 and then placed in a cracking reactor, and cracked at 300~400°C for 1~5h. After the reaction, the reaction raw materials are filtered out, and the The lysate is transferred into a distillation pot for distillation treatment, and the fractions at 40-190°C are collected as gasoline components, and the fractions at 250-330°C are collected as diesel oil.
CN201210336113.XA 2012-09-12 2012-09-12 Method for preparing fuel oil from waste paper waste residue Expired - Fee Related CN102911690B (en)

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CN104593036A (en) * 2015-01-06 2015-05-06 珠海市盈润环保科技有限公司 Regenerated fuel oil extracted from waste filter cakes for producing sulfonate and preparation method of regenerated fuel oil
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CN108079992B (en) * 2016-11-21 2020-07-14 北京华石联合能源科技发展有限公司 Preparation method and application of combined catalyst
CN108079995B (en) * 2016-11-21 2021-04-06 北京华石联合能源科技发展有限公司 Combined catalyst and application
CN108080004B (en) * 2016-11-21 2021-04-06 北京华石联合能源科技发展有限公司 Hydrogenation catalyst composition and application thereof
JP6883830B1 (en) * 2020-06-25 2021-06-09 株式会社アクト Organic waste recycling equipment and its recycling method
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