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CN107043656A - A kind of dispersant and wash mill for being used to wash sial phosphorus molecular sieve - Google Patents

A kind of dispersant and wash mill for being used to wash sial phosphorus molecular sieve Download PDF

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Publication number
CN107043656A
CN107043656A CN201710281436.6A CN201710281436A CN107043656A CN 107043656 A CN107043656 A CN 107043656A CN 201710281436 A CN201710281436 A CN 201710281436A CN 107043656 A CN107043656 A CN 107043656A
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molecular sieve
solution
phosphorus molecular
solvent
kettle
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CN107043656B (en
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李欢
王聪
刘新伟
王海国
王翔
白世杰
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China Tianchen Engineering Corp
Tianjin Tianchen Green Energy Resources Engineering Technology and Development Co Ltd
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Tianjin Tianchen Green Energy Resources Engineering Technology and Development Co Ltd
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    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
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    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J29/00Catalysts comprising molecular sieves
    • B01J29/82Phosphates
    • B01J29/84Aluminophosphates containing other elements, e.g. metals, boron
    • B01J29/85Silicoaluminophosphates [SAPO compounds]
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/06Washing
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    • C07C2/00Preparation of hydrocarbons from hydrocarbons containing a smaller number of carbon atoms
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    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
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    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00Other compounding ingredients of detergent compositions covered in group C11D1/00
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    • C11D3/2072Aldehydes-ketones
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    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00Other compounding ingredients of detergent compositions covered in group C11D1/00
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    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00Other compounding ingredients of detergent compositions covered in group C11D1/00
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    • C11D3/00Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/16Organic compounds
    • C11D3/37Polymers
    • C11D3/3746Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
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    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
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    • C11D3/00Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/43Solvents
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract

本发明提供了一种用于洗涤硅铝磷分子筛的分散剂及洗涤装置,该分散剂包括按照质量(0.01‑0.3):1混合的溶液A和溶液B;所述溶液A包括溶剂醇类,溶质为盐酸、硬脂酰胺或硬脂甘油酯或二者的混合物、三硬脂酸甘油酯;所述溶液B包括溶剂脱盐水,溶质为甲醛、聚乙烯醇、聚丙烯酸钠或烷基磺酸钠或二者的混合物。用于洗涤硅铝磷分子筛的装置,包括压滤机、螺旋输送机以及打浆釜、离心泵、收料斗、喷淋装置等。本发明避免了压滤后的硅铝磷分子筛在管道或设备上发生结块堵塞的情况,更加快速的洗涤硅铝磷分子筛的同时,不仅提高了洗涤硅铝磷分子筛的效率,也降低了脱盐水的40‑70%的使用量,自动化程度高,便于工业化推广。

The invention provides a dispersant and a washing device for washing silicon-aluminum-phosphorus molecular sieves, the dispersant includes solution A and solution B mixed according to mass (0.01-0.3): 1; the solution A includes solvent alcohols, The solute is hydrochloric acid, stearamide or stearyl glyceride or a mixture of the two, glyceryl tristearate; the solution B includes solvent desalted water, and the solute is formaldehyde, polyvinyl alcohol, sodium polyacrylate or alkylsulfonic acid Sodium or a mixture of both. The device used for washing silicon aluminum phosphorus molecular sieve, including filter press, screw conveyor, beating kettle, centrifugal pump, receiving hopper, spraying device, etc. The invention avoids the agglomeration and clogging of the silicon-aluminum-phosphorus molecular sieve after press filtration on the pipeline or equipment, and while washing the silicon-aluminum-phosphorus molecular sieve more quickly, it not only improves the washing efficiency of the silicon-aluminum-phosphorus molecular sieve, but also reduces desalination 40-70% of the water consumption, high degree of automation, easy to promote industrialization.

Description

一种用于洗涤硅铝磷分子筛的分散剂及洗涤装置Dispersant and washing device for washing silicon aluminum phosphorus molecular sieve

技术领域technical field

本发明属于化工技术领域,尤其是涉及一种用于洗涤硅铝磷分子筛的分散剂及洗涤装置。The invention belongs to the technical field of chemical industry, and in particular relates to a dispersant and a washing device for washing silicon-aluminum-phosphorous molecular sieves.

背景技术Background technique

丙烯是目前世界上最重要的大宗化工产品和支撑我国经济发展的基础化工原料之一,可制备多种基本有机原料。例如可制备环氧丙烷、丙烯醛、丙烯醇、异丙醇、四氯化碳、丁醇等等。近年来,由于受下游衍生物(尤其是聚丙烯)需求的影响,丙烯的需求量大幅增大。由于国内丙烯资源的短缺,远远不能满足国内市场的需求,国内自给率大幅下降,需要大量进口。随着国际市场激烈竞争的环境,发展丙烯及其衍生物必须采用国际上最先进的环境友好工艺技术,达到低成本生产的大型经济规模,中国丙烯的开发利用前景很是广阔。Propylene is currently the most important bulk chemical product in the world and one of the basic chemical raw materials supporting my country's economic development. It can be used to prepare a variety of basic organic raw materials. For example, propylene oxide, acrolein, propenyl alcohol, isopropanol, carbon tetrachloride, butanol and the like can be prepared. In recent years, due to the demand for downstream derivatives (especially polypropylene), the demand for propylene has increased significantly. Due to the shortage of domestic propylene resources, it is far from meeting the needs of the domestic market, and the domestic self-sufficiency rate has dropped sharply, requiring a large amount of imports. With the environment of fierce competition in the international market, the development of propylene and its derivatives must adopt the most advanced environmentally friendly technology in the world to achieve large-scale economical production at low cost. The prospect of development and utilization of propylene in China is very broad.

针对中国丙烯发展前景,中国天辰工程有限公司研制的甲醇制丙烯催化剂主要是一种硅铝磷分子筛,这种分子筛能够使甲醇转化率达到100%或者接近100%,乙烯和丙烯的选择性在78%以上,几乎没有C5以上的产物,而且硅铝磷分子筛突出的水热稳定性和适宜的孔道结构使其性能更加优越,必将成为日后得到广泛应用。Aiming at the prospect of propylene development in China, the methanol-to-propylene catalyst developed by China Tianchen Engineering Co., Ltd. is mainly a silicon-aluminum-phosphorus molecular sieve, which can make the methanol conversion rate reach 100% or close to 100%, and the selectivity of ethylene and propylene is at 78 % or more, there are almost no products above C5, and the outstanding hydrothermal stability and suitable pore structure of the silicon-aluminum-phosphorus molecular sieve make it more superior in performance, and will be widely used in the future.

目前,有关清洗分子筛等物料的装置和方法很多,具体涉及到的只有离心洗涤、板框过滤洗涤、压滤机洗涤等。在物料通过洗涤方式除去分子筛浆液中的溶胶、有机质等杂质时,物料会在过滤机内挤压成型后结块,结块现象容易聚积成坚硬的大块,影响输送与打浆过程,同时未洗涤干净的硅铝磷分子筛具有粘性,附着在管道与螺旋输送机上,造成设备及管道堵塞,对现场操作造成阻碍,清洗管道和设备也比较麻烦。此外,对于洗涤分子筛需要大量的脱盐水,对于水资源短缺的地方非常不利。因此,针对硅铝磷分子筛,寻求一种安全可靠的解决物料结块,粘在管道和装置上的问题方法,同时可循环使用洗涤液从而节约用水的技术,成为了目前该领域亟待解决的问题。At present, there are many devices and methods for cleaning materials such as molecular sieves, and only centrifugal washing, plate and frame filter washing, and filter press washing are specifically involved. When the material is washed to remove impurities such as sol and organic matter in the molecular sieve slurry, the material will be agglomerated after being extruded in the filter, and the agglomeration phenomenon will easily accumulate into hard chunks, which will affect the transportation and beating process. The clean silicon-aluminum-phosphorus molecular sieve is viscous and adheres to pipelines and screw conveyors, causing blockage of equipment and pipelines, hindering on-site operations, and troublesome cleaning of pipelines and equipment. In addition, a large amount of desalted water is required for washing molecular sieves, which is very unfavorable for places where water resources are scarce. Therefore, for silicon-aluminum-phosphorus molecular sieves, seeking a safe and reliable solution to the problem of material agglomeration and sticking to pipes and devices, and at the same time recycling the washing liquid to save water has become an urgent problem in this field. .

发明内容Contents of the invention

有鉴于此,本发明旨在提出一种用于洗涤硅铝磷分子筛的分散剂及洗涤装置,以解决物料结块,粘在管道和装置上的问题,同时可循环使用洗涤液从而达到节约用水的技术。In view of this, the present invention aims to propose a dispersant and washing device for washing silicon-aluminum-phosphorus molecular sieves to solve the problem of material agglomeration and sticking to pipes and devices, and at the same time, the washing liquid can be recycled to save water Technology.

为达到上述目的,本发明的技术方案是这样实现的:In order to achieve the above object, technical solution of the present invention is achieved in that way:

一种用于洗涤硅铝磷分子筛的分散剂,包括按照质量比(0.01-0.3):1混合的溶液A和溶液B;A dispersant for washing silicon-aluminum-phosphorus molecular sieves, comprising solution A and solution B mixed according to mass ratio (0.01-0.3): 1;

所述溶液A包括溶剂,溶剂质量的3-10%的盐酸,溶剂质量的0.3-0.8%的硬脂酰胺或硬脂甘油酯或二者的混合物;溶剂质量的14-32%的三硬脂酸甘油酯;Described solution A comprises solvent, the hydrochloric acid of 3-10% of solvent quality, the stearamide or stearyl glyceride of 0.3-0.8% of solvent quality or the mixture of both; The tristearic acid of 14-32% of solvent quality glycerides;

所述溶液B包括溶剂,溶剂质量的0.01-0.03%的甲醛,溶剂质量的0-15%的聚乙烯醇,溶剂质量的0-8%的聚丙烯酸钠或烷基磺酸钠或二者的混合物;Said solution B comprises solvent, 0.01-0.03% formaldehyde of solvent quality, 0-15% polyvinyl alcohol of solvent quality, 0-8% of solvent quality sodium polyacrylate or sodium alkylsulfonate or both mixture;

溶液A的溶剂为醇;溶液B的溶剂为脱盐水。The solvent of solution A is alcohol; the solvent of solution B is desalted water.

优选的,所述醇为甲醇、乙醇、丙二醇、丙三醇、正丁醇、异丁醇、苯甲醇、乙二醇一种或两种;所述脱盐水的电导率小于5μS/cm,pH为6.0~7.0。Preferably, the alcohol is one or two of methanol, ethanol, propylene glycol, glycerol, n-butanol, isobutanol, benzyl alcohol, and ethylene glycol; the conductivity of the desalted water is less than 5 μS/cm, and the pH 6.0 to 7.0.

优选的,溶液A的制备包括如下步骤,(1)选用30-60℃的醇作为溶剂,此外加入溶剂质量的3-10%的盐酸搅拌均匀;(2)添加相当于溶剂质量的0.3-0.8%的硬脂酰胺或硬脂甘油酯或二者的混合物;(3)添加相当于溶剂质量的14-32%的三硬脂酸甘油酯,混合均匀;Preferably, the preparation of solution A includes the following steps: (1) select alcohol at 30-60° C. as the solvent, and add 3-10% hydrochloric acid of the mass of the solvent and stir evenly; (2) add 0.3-0.8% of the mass of the solvent % stearamide or stearyl glyceride or the mixture of the two; (3) add glyceryl tristearate equivalent to 14-32% of the solvent quality, and mix homogeneously;

溶液B的制备包括如下步骤,(1)选用脱盐水作为溶剂,此外添加0.01-0.03%的甲醛搅拌均匀;(2)添加相当于溶剂质量的0-15%的聚乙烯醇;(3)添加相当于溶剂质量的0-8%的聚丙烯酸钠或烷基磺酸钠或二者的混合物,混合均匀。The preparation of solution B includes the following steps: (1) select desalted water as the solvent, add 0.01-0.03% formaldehyde and stir evenly; (2) add polyvinyl alcohol equivalent to 0-15% of the solvent mass; (3) add Sodium polyacrylate or sodium alkylsulfonate or a mixture of the two, which is equivalent to 0-8% of the mass of the solvent, is mixed evenly.

本发明同时提供一种循环洗涤硅铝磷分子筛的装置,包括压滤机、螺旋输送机以及打浆釜;所述压滤机与打浆釜通过管道连通,且管道上设有第一阀门以及离心泵;所述螺旋输送机上设有收料斗,所述收料斗位于压滤机的出口下方;所述螺旋输送机的两个出口分别连接产品罐以及打浆釜;所述收料斗上方设有喷淋装置,所述喷淋装置与打浆釜之间通过管道连通,且管道上设有第二阀门以及离心泵。The present invention also provides a device for circularly washing silicon-aluminum-phosphorus molecular sieves, including a filter press, a screw conveyor, and a beating kettle; the filter press and the beating kettle are connected through a pipeline, and the pipeline is provided with a first valve and a centrifugal pump ; The screw conveyor is provided with a receiving hopper, and the receiving hopper is located below the outlet of the filter press; the two outlets of the screw conveyor are respectively connected to the product tank and the beating kettle; the top of the receiving hopper is provided with a spraying device , the spraying device communicates with the beating kettle through a pipeline, and the pipeline is provided with a second valve and a centrifugal pump.

优选的,所述打浆釜底端连接有循环总管,所述循环总管分支出两个分管,分别与压滤机以及喷淋装置连通,且分管上分别设有第一阀门以及第二阀门;在循环总管上设有离心泵。Preferably, the bottom end of the beating kettle is connected with a circulation main pipe, and the circulation main pipe is branched into two branch pipes, which communicate with the filter press and the spraying device respectively, and the branch pipes are respectively provided with a first valve and a second valve; A centrifugal pump is arranged on the circulation main pipe.

本发明还提供了一种使用如上所述的装置洗涤循环洗涤硅铝磷分子筛的方法,其特征在于:包括如下步骤,The present invention also provides a method for washing silicon-aluminum-phosphorous molecular sieves using the above-mentioned device washing cycle, which is characterized in that: it includes the following steps,

1)向打浆釜内注入如上所述的分散剂,且分散剂的质量为待洗涤硅铝分子筛质量的0.5-2%;之后向打浆釜内注入打浆釜容积40~75%的脱盐水作为初始洗涤液,搅拌,并开启离心泵,使洗涤液经管道从收料斗的上方的喷淋装置均匀喷出;1) Inject the above-mentioned dispersant into the beating kettle, and the quality of the dispersant is 0.5-2% of the mass of the silica-alumina molecular sieve to be washed; then inject desalted water of 40-75% of the volume of the beating kettle into the beating kettle as the initial Stir the washing liquid, and turn on the centrifugal pump, so that the washing liquid is evenly sprayed from the spray device above the receiving hopper through the pipeline;

2)合成的新鲜硅铝磷分子筛浆液进入压滤机中压滤,压滤后的硅铝磷分子筛掉入收料斗,硅铝磷分子筛经喷淋的洗涤液润湿后,被双螺旋输送机输送到打浆釜中形成新混合液;2) The synthesized fresh Si-Al-P molecular sieve slurry enters the filter press for pressure filtration, and the Si-Al-P molecular sieve after pressure filtration falls into the receiving hopper. Transport to the beating tank to form a new mixed liquor;

3)压滤机压滤完新鲜的硅铝磷分子筛浆液后,打开第一阀门,调节离心泵,同时向打浆釜内连续通入脱盐水,打浆釜内的新混合液一部分经管道进入压滤机进行压滤,压滤出的液体排出压滤机,压滤出的滤饼再次进入收料斗;另一部分的新混合液经喷淋装置对收料斗内的硅铝分子筛进行润湿,润湿后的硅铝磷分子筛再次被双螺旋输送机输送到打浆釜内;进入压滤机新混合液与进入喷淋装置的新混合液的体积比为(20-40):1;3) After the fresh silicon aluminum phosphorus molecular sieve slurry is filtered by the filter press, the first valve is opened, the centrifugal pump is adjusted, and desalted water is continuously fed into the beating kettle at the same time, and a part of the new mixed solution in the beating kettle enters the press filter through the pipeline The press filter is carried out, the liquid out of the press filter is discharged out of the filter press, and the filter cake out of the press filter enters the hopper again; the other part of the new mixed liquid is wetted by the spray device to the silicon-aluminum molecular sieve in the hopper, and the wetting The silicon-aluminum-phosphorus molecular sieve is transported to the beating kettle again by the double-screw conveyor; the volume ratio of the new mixed solution entering the filter press and the new mixed solution entering the spraying device is (20-40):1;

4)重复步骤2)以及步骤3)共2-5次,当打浆釜内的溶液pH为6.6~8.2,则关闭第二阀门,停止向打浆釜通入脱盐水,同时双螺旋输送机逆向旋转,把压滤机压滤出的滤饼输送到产品罐中。4) Repeat step 2) and step 3) for a total of 2-5 times. When the pH of the solution in the beating kettle is 6.6-8.2, close the second valve, stop feeding desalted water into the beating kettle, and at the same time, the double-screw conveyor rotates in reverse , to transport the filter cake from the filter press to the product tank.

优选的,还包括步骤5),打开第一阀门和第二阀门,向打浆釜内通入脱盐水,调节双螺旋输送机旋转,通过脱盐水的循环对整个装置体系进行清洗。Preferably, step 5) is also included, opening the first valve and the second valve, feeding desalted water into the beating tank, adjusting the rotation of the double screw conveyor, and cleaning the entire device system through the circulation of desalinated water.

优选的,在整个循环洗涤时,打浆釜内的混合液中,硅铝磷分子筛的固含量低于34%。Preferably, during the whole washing cycle, the solid content of the silicon-aluminum-phosphorus molecular sieve in the mixed liquid in the beating tank is lower than 34%.

优选的,通入到打浆釜内的脱盐水流量始终使打浆釜内的液位保持在50~75%之间;管道的口径为50~90mm。Preferably, the flow of desalted water into the beating kettle keeps the liquid level in the beating kettle between 50-75%; the diameter of the pipeline is 50-90mm.

优选的,压滤机单次处理的合成的新鲜硅铝磷分子筛浆液的体积为打浆釜内洗涤液体积的50-180%。Preferably, the volume of the fresh silicon-aluminum-phosphorus molecular sieve slurry processed once by the filter press is 50-180% of the volume of the washing liquid in the beating tank.

相对于现有技术,本发明所述的分散剂以及洗涤装置,具有以下优势:Compared with the prior art, the dispersant and washing device of the present invention have the following advantages:

本发明提供的分散剂以及洗涤装置,避免了压滤后的硅铝磷分子筛在管道或设备上发生结块堵塞的情况,不仅提高了洗涤硅铝磷分子筛的效率,也降低了脱盐水的40-70%的使用量,自动化程度高,便于工业化推广。The dispersant and washing device provided by the present invention avoid the clogging and clogging of the silicon aluminum phosphorus molecular sieve after pressure filtration on the pipeline or equipment, not only improve the washing efficiency of the silicon aluminum phosphorus molecular sieve, but also reduce the 40% of the desalted water -70% usage, high degree of automation, convenient for industrial promotion.

附图说明Description of drawings

构成本发明的一部分的附图用来提供对本发明的进一步理解,本发明的示意性实施例及其说明用于解释本发明,并不构成对本发明的不当限定。在附图中:The drawings constituting a part of the present invention are used to provide a further understanding of the present invention, and the schematic embodiments and descriptions of the present invention are used to explain the present invention, and do not constitute an improper limitation of the present invention. In the attached picture:

图1为本发明实施例所述的洗涤装置的简单结构示意图;Fig. 1 is the simple structure diagram of the washing device described in the embodiment of the present invention;

附图标记说明:Explanation of reference signs:

1-压滤机,2-收料斗,3-打浆釜,4-螺旋输送机,5-产品罐,6-循环总管,7-分管,8-第一阀门,9-第二阀门;10-离心泵;11-喷淋装置。1-Filter press, 2-Hopper, 3-Beating kettle, 4-Screw conveyor, 5-Product tank, 6-Circulation main pipe, 7-Branch pipe, 8-First valve, 9-Second valve; 10- Centrifugal pump; 11-spraying device.

具体实施方式detailed description

需要说明的是,在不冲突的情况下,本发明中的实施例及实施例中的特征可以相互组合。It should be noted that, in the case of no conflict, the embodiments of the present invention and the features in the embodiments can be combined with each other.

一种循环洗涤硅铝磷分子筛的装置,其特征在于:包括压滤机1、螺旋输送机4以及打浆釜3;所述压滤机1与打浆釜3通过管道连通,且管道上设有第一阀门8以及离心泵10;所述螺旋输送机4上设有收料斗2,所述收料斗2位于压滤机1的出口下方;所述螺旋输送机4的两个出口分别连接产品罐5以及打浆釜3;所述收料斗2上方设有喷淋装置11,所述喷淋装置11与打浆釜3之间通过管道连通,且管道上设有第二阀门9以及离心泵10。A device for circularly washing silicon-aluminum-phosphorus molecular sieves, characterized in that: it includes a filter press 1, a screw conveyor 4 and a beating kettle 3; the filter press 1 and the beating kettle 3 are connected through a pipeline, and the pipeline is provided with a first A valve 8 and a centrifugal pump 10; the screw conveyor 4 is provided with a receiving hopper 2, and the receiving hopper 2 is located below the outlet of the filter press 1; the two outlets of the screw conveyor 4 are respectively connected to the product tank 5 And the beating kettle 3; a spraying device 11 is arranged above the receiving hopper 2, and the spraying device 11 is connected with the beating kettle 3 through a pipeline, and a second valve 9 and a centrifugal pump 10 are arranged on the pipeline.

所述压滤机1与打浆釜3通过管道连通,以及连通喷淋装置11与打浆釜3的管道,可以是单独的两个管道,也可以采用以下方式:The filter press 1 is communicated with the beating kettle 3 through pipelines, and the pipeline connecting the spraying device 11 and the beating kettle 3 can be two independent pipelines, and the following methods can also be adopted:

所述打浆釜3底端连接有循环总管6,所述循环总管6分支出两个分管7,分别与压滤机1以及喷淋装置11连通,且两个分管7上分别设有第一阀门8以及第二阀门9;在循环总管6上设有离心泵10。The bottom end of the beating kettle 3 is connected with a circulation main pipe 6, and the circulation main pipe 6 is branched into two sub-pipes 7, which communicate with the filter press 1 and the spraying device 11 respectively, and the two sub-pipes 7 are respectively provided with first valves 8 and the second valve 9; a centrifugal pump 10 is provided on the circulation main pipe 6.

实施例一Embodiment one

一种用于洗涤硅铝磷分子筛的分散剂,包括按照质量比0.05:1混合的溶液A和溶液B;A dispersant for washing silicon-aluminum-phosphorus molecular sieves, comprising solution A and solution B mixed in a mass ratio of 0.05:1;

所述溶液A包括溶剂,溶剂质量的4%的盐酸,溶剂质量的0.4%的硬脂酰胺或硬脂甘油酯或二者的混合物;溶剂质量的16%的三硬脂酸甘油酯;Said solution A comprises solvent, 4% hydrochloric acid of solvent mass, 0.4% stearamide or stearyl glyceride or the mixture of the two; 16% tristearin of solvent mass;

所述溶液B包括溶剂,溶剂质量的0.01%的甲醛,溶剂质量的4%的聚乙烯醇,溶剂质量的3%的聚丙烯酸钠或烷基磺酸钠或二者的混合物;Said solution B comprises solvent, 0.01% formaldehyde of solvent mass, 4% polyvinyl alcohol of solvent mass, 3% sodium polyacrylate or sodium alkylsulfonate or a mixture of the two;

溶液A的溶剂为醇;溶液B的溶剂为脱盐水。The solvent of solution A is alcohol; the solvent of solution B is desalted water.

所述醇为甲醇;所述脱盐水的电导率为2μS/cm,pH为6.7。The alcohol is methanol; the conductivity of the desalted water is 2 μS/cm, and the pH is 6.7.

溶液A的制备包括如下步骤,(1)选用40℃的醇作为溶剂,此外加入盐酸搅拌均匀;(2)添加硬脂酰胺或硬脂甘油酯或二者的混合物;(3)添加三硬脂酸甘油酯,混合均匀;The preparation of solution A includes the following steps: (1) select alcohol at 40°C as the solvent, add hydrochloric acid and stir evenly; (2) add stearamide or stearyl glyceride or a mixture of the two; (3) add tristearyl Glycerides, mixed evenly;

溶液B的制备包括如下步骤,(1)选用脱盐水作为溶剂,此外添加甲醛搅拌均匀;(2)添加聚乙烯醇;(3)添加聚丙烯酸钠或烷基磺酸钠或二者的混合物,混合均匀。The preparation of solution B comprises the following steps, (1) select desalted water as the solvent, add formaldehyde and stir evenly; (2) add polyvinyl alcohol; (3) add sodium polyacrylate or sodium alkylsulfonate or a mixture of the two, well mixed.

一种使用如上所述装置洗涤循环洗涤硅铝磷分子筛的方法,包括如下步骤,A method for washing silicon-aluminum-phosphorous molecular sieves using the washing cycle of the above-mentioned device, comprising the following steps,

1)向打浆釜内注入分散剂,且分散剂的质量为待洗涤硅铝分子筛质量的0.8%;之后向打浆釜内注入打浆釜容积60%的脱盐水作为初始洗涤液,搅拌,并开启离心泵,使洗涤液经管道从收料斗的上方的喷淋装置均匀喷出;1) Inject a dispersant into the beating kettle, and the quality of the dispersant is 0.8% of the mass of the silica-alumina molecular sieve to be washed; then inject desalted water of 60% of the volume of the beating kettle into the beating kettle as the initial washing liquid, stir, and start the centrifuge Pump, so that the washing liquid is evenly sprayed from the spray device above the receiving hopper through the pipeline;

2)合成的新鲜硅铝磷分子筛浆液进入压滤机中压滤,压滤后的硅铝磷分子筛掉入收料斗,硅铝磷分子筛经喷淋的洗涤液润湿后,被双螺旋输送机输送到打浆釜中形成新混合液;2) The synthesized fresh Si-Al-P molecular sieve slurry enters the filter press for pressure filtration, and the Si-Al-P molecular sieve after pressure filtration falls into the receiving hopper. Transport to the beating tank to form a new mixed liquor;

3)压滤机压滤完新鲜的硅铝磷分子筛浆液后,打开第一阀门,调节离心泵,同时向打浆釜内连续通入脱盐水,打浆釜内的新混合液一部分经管道进入压滤机进行压滤,压滤出的液体排出压滤机,压滤出的滤饼再次进入收料斗;另一部分的新混合液经喷淋装置对收料斗内的硅铝分子筛进行润湿,润湿后的硅铝磷分子筛再次被双螺旋输送机输送到打浆釜内;进入压滤机新混合液与进入喷淋装置的新混合液的体积比为20:1;3) After the fresh silicon aluminum phosphorus molecular sieve slurry is filtered by the filter press, the first valve is opened, the centrifugal pump is adjusted, and desalted water is continuously fed into the beating kettle at the same time, and a part of the new mixed solution in the beating kettle enters the press filter through the pipeline The press filter is carried out, the liquid out of the press filter is discharged out of the filter press, and the filter cake out of the press filter enters the hopper again; the other part of the new mixed liquid is wetted by the spray device to the silicon-aluminum molecular sieve in the hopper, and the wetting The finished silicon aluminum phosphorus molecular sieve is transported to the beating kettle again by the double screw conveyor; the volume ratio of the new mixed liquid entering the filter press and the new mixed liquid entering the spraying device is 20:1;

4)重复步骤2)以及步骤3)共3次,当打浆釜内的溶液pH为7.6,则关闭第二阀门,停止向打浆釜通入脱盐水,同时双螺旋输送机逆向旋转,把压滤机压滤出的滤饼输送到产品罐中。4) Repeat step 2) and step 3) for a total of 3 times. When the pH of the solution in the beating kettle is 7.6, close the second valve, stop feeding desalted water into the beating kettle, and at the same time, the double screw conveyor rotates in reverse to filter the press filter. The filter cake filtered by machine pressure is conveyed to the product tank.

5)打开第一阀门和第二阀门,向打浆釜内通入脱盐水,调节双螺旋输送机旋转,通过脱盐水的循环对整个装置体系进行清洗。5) Open the first valve and the second valve, pass desalted water into the beating tank, adjust the rotation of the double screw conveyor, and clean the entire device system through the circulation of desalinated water.

在整个循环洗涤时,打浆釜内的混合液中,硅铝磷分子筛的固含量在21%左右。During the whole cycle of washing, the solid content of the silicon-aluminum-phosphorus molecular sieve in the mixed liquid in the beating kettle is about 21%.

通入到打浆釜内的脱盐水流量始终使打浆釜内的液位保持在60~65%之间;管道的口径为72mm。The flow rate of desalted water fed into the beating kettle keeps the liquid level in the beating kettle between 60% and 65%; the diameter of the pipeline is 72mm.

压滤机单次处理的合成的新鲜硅铝磷分子筛浆液的体积为打浆釜内洗涤液体积的100%。The volume of the fresh silicon-aluminum-phosphorus molecular sieve slurry processed once by the filter press is 100% of the volume of the washing liquid in the beating kettle.

实施例二Embodiment two

一种用于洗涤硅铝磷分子筛的分散剂,包括按照体积比0.18:1混合的溶液A和溶液B;A dispersant for washing silicon-aluminum-phosphorus molecular sieves, comprising solution A and solution B mixed at a volume ratio of 0.18:1;

所述溶液A包括溶剂,溶剂质量的6%的盐酸,溶剂质量的0.6%的硬脂酰胺或硬脂甘油酯或二者的混合物;溶剂质量的20%的三硬脂酸甘油酯;Said solution A comprises solvent, 6% hydrochloric acid of solvent mass, 0.6% stearamide or stearyl glyceride or the mixture of both; 20% tristearin of solvent mass;

所述溶液B包括溶剂,溶剂质量的0.02%的甲醛,溶剂质量的6%的聚乙烯醇,溶剂质量的4%的聚丙烯酸钠或烷基磺酸钠或二者的混合物;Said solution B comprises solvent, 0.02% formaldehyde of solvent mass, 6% polyvinyl alcohol of solvent mass, 4% sodium polyacrylate or sodium alkylsulfonate or a mixture of the two;

溶液A的溶剂为醇;溶液B的溶剂为脱盐水。The solvent of solution A is alcohol; the solvent of solution B is desalted water.

所述醇为乙醇;所述脱盐水的电导率4μS/cm,pH为6.0。The alcohol is ethanol; the conductivity of the desalted water is 4 μS/cm, and the pH is 6.0.

溶液A的制备包括如下步骤,(1)选用50℃的醇作为溶剂,此外加入盐酸搅拌均匀;(2)添加硬脂酰胺或硬脂甘油酯或二者的混合物;(3)添加三硬脂酸甘油酯,混合均匀;The preparation of solution A includes the following steps: (1) select alcohol at 50°C as the solvent, add hydrochloric acid and stir evenly; (2) add stearamide or stearyl glyceride or a mixture of the two; (3) add tristearyl Glycerides, mixed evenly;

溶液B的制备包括如下步骤,(1)选用脱盐水作为溶剂,此外添加甲醛搅拌均匀;(2)添加聚乙烯醇;(3)添加聚丙烯酸钠或烷基磺酸钠或二者的混合物,混合均匀。The preparation of solution B comprises the following steps, (1) select desalted water as the solvent, add formaldehyde and stir evenly; (2) add polyvinyl alcohol; (3) add sodium polyacrylate or sodium alkylsulfonate or a mixture of the two, well mixed.

一种使用如上所述装置洗涤循环洗涤硅铝磷分子筛的方法,包括如下步骤,A method for washing silicon-aluminum-phosphorous molecular sieves using the washing cycle of the above-mentioned device, comprising the following steps,

1)向打浆釜内注入分散剂,且分散剂的质量为待洗涤硅铝分子筛质量的1.5%;之后向打浆釜内注入打浆釜容积55%的脱盐水作为初始洗涤液,搅拌,并开启离心泵,使洗涤液经管道从收料斗的上方的喷淋装置均匀喷出;1) Inject a dispersant into the beating kettle, and the quality of the dispersant is 1.5% of the mass of the silica-alumina molecular sieve to be washed; then inject desalted water with 55% of the volume of the beating kettle into the beating kettle as the initial washing liquid, stir, and start the centrifuge Pump, so that the washing liquid is evenly sprayed from the spray device above the receiving hopper through the pipeline;

2)合成的新鲜硅铝磷分子筛浆液进入压滤机中压滤,压滤后的硅铝磷分子筛掉入收料斗,硅铝磷分子筛经喷淋的洗涤液润湿后,被双螺旋输送机输送到打浆釜中形成新混合液;2) The synthesized fresh Si-Al-P molecular sieve slurry enters the filter press for pressure filtration, and the Si-Al-P molecular sieve after pressure filtration falls into the receiving hopper. Transport to the beating tank to form a new mixed liquor;

3)压滤机压滤完新鲜的硅铝磷分子筛浆液后,打开第一阀门,调节离心泵,同时向打浆釜内连续通入脱盐水,打浆釜内的新混合液一部分经管道进入压滤机进行压滤,压滤出的液体排出压滤机,压滤出的滤饼再次进入收料斗;另一部分的新混合液经喷淋装置对收料斗内的硅铝分子筛进行润湿,润湿后的硅铝磷分子筛再次被双螺旋输送机输送到打浆釜内;进入压滤机新混合液与进入喷淋装置的新混合液的体积比为25:1;3) After the fresh silicon aluminum phosphorus molecular sieve slurry is filtered by the filter press, the first valve is opened, the centrifugal pump is adjusted, and desalted water is continuously fed into the beating kettle at the same time, and a part of the new mixed solution in the beating kettle enters the press filter through the pipeline The press filter is carried out, the liquid out of the press filter is discharged out of the filter press, and the filter cake out of the press filter enters the hopper again; the other part of the new mixed liquid is wetted by the spray device to the silicon-aluminum molecular sieve in the hopper, and the wetting The finished silicon aluminum phosphorus molecular sieve is transported to the beating kettle again by the double screw conveyor; the volume ratio of the new mixed solution entering the filter press and the new mixed solution entering the spraying device is 25:1;

4)重复步骤2)以及步骤3)共4次当打浆釜内的溶液pH为7.8,则关闭第二阀门,停止向打浆釜通入脱盐水,同时双螺旋输送机逆向旋转,把压滤机压滤出的滤饼输送到产品罐中。4) Repeat step 2) and step 3) for a total of 4 times. When the pH of the solution in the beating kettle is 7.8, close the second valve and stop feeding desalted water into the beating kettle. The press-filtered filter cake is conveyed to the product tank.

5)打开第一阀门和第二阀门,向打浆釜内通入脱盐水,调节双螺旋输送机旋转,通过脱盐水的循环对整个装置体系进行清洗。5) Open the first valve and the second valve, pass desalted water into the beating tank, adjust the rotation of the double screw conveyor, and clean the entire device system through the circulation of desalinated water.

在整个循环洗涤时,打浆釜内的混合液中,硅铝磷分子筛的固含量在30%左右。During the whole cycle of washing, the solid content of the silicon aluminum phosphorus molecular sieve in the mixed liquid in the beating kettle is about 30%.

通入到打浆釜内的脱盐水流量始终使打浆釜内的液位保持在70%之间;管道的口径为72mm。The flow of desalted water into the beating kettle keeps the liquid level in the beating kettle between 70%; the diameter of the pipeline is 72mm.

压滤机单次处理的合成的新鲜硅铝磷分子筛浆液的体积为打浆釜内洗涤液体积的140%。The volume of the synthesized fresh silicon-aluminum-phosphorus molecular sieve slurry treated once by the filter press is 140% of the volume of the washing liquid in the beating kettle.

实施例三Embodiment three

一种用于洗涤硅铝磷分子筛的分散剂,包括按照体积比0.28:1混合的溶液A和溶液B;A dispersant for washing silicon-aluminum-phosphorus molecular sieves, comprising solution A and solution B mixed at a volume ratio of 0.28:1;

所述溶液A包括溶剂,溶剂质量的8%的盐酸,溶剂质量的0.7%的硬脂酰胺或硬脂甘油酯或二者的混合物;溶剂质量的28%的三硬脂酸甘油酯;Described solution A comprises solvent, the hydrochloric acid of 8% of solvent quality, the stearyl amide or stearyl glyceride of 0.7% of solvent quality or the mixture of both; The glyceryl tristearate of 28% of solvent quality;

所述溶液B包括溶剂,溶剂质量的0.03%的甲醛,溶剂质量的13%的聚乙烯醇,溶剂质量的7%的聚丙烯酸钠或烷基磺酸钠或二者的混合物;Said solution B comprises solvent, 0.03% formaldehyde of solvent mass, 13% polyvinyl alcohol of solvent mass, 7% sodium polyacrylate or sodium alkyl sulfonate or the mixture of both;

溶液A的溶剂为醇;溶液B的溶剂为脱盐水。The solvent of solution A is alcohol; the solvent of solution B is desalted water.

所述醇为甲醇;所述脱盐水的电导率为2μS/cm,pH为7.0。The alcohol is methanol; the conductivity of the desalted water is 2 μS/cm, and the pH is 7.0.

溶液A的制备包括如下步骤,(1)选用55℃的醇作为溶剂,此外加入盐酸搅拌均匀;(2)添加硬脂酰胺或硬脂甘油酯或二者的混合物;(3)添加三硬脂酸甘油酯,混合均匀;The preparation of solution A includes the following steps: (1) select alcohol at 55°C as the solvent, add hydrochloric acid and stir evenly; (2) add stearamide or stearyl glyceride or a mixture of the two; (3) add tristearyl Glycerides, mixed evenly;

溶液B的制备包括如下步骤,(1)选用脱盐水作为溶剂,此外添加甲醛搅拌均匀;(2)添加聚乙烯醇;(3)添加聚丙烯酸钠或烷基磺酸钠或二者的混合物,混合均匀。The preparation of solution B comprises the following steps, (1) select desalted water as the solvent, add formaldehyde and stir evenly; (2) add polyvinyl alcohol; (3) add sodium polyacrylate or sodium alkylsulfonate or a mixture of the two, well mixed.

一种使用如上所述装置洗涤循环洗涤硅铝磷分子筛的方法,包括如下步骤,A method for washing silicon-aluminum-phosphorous molecular sieves using the washing cycle of the above-mentioned device, comprising the following steps,

1)向打浆釜内注入分散剂,且分散剂的质量为待洗涤硅铝分子筛质量的1.8%;之后向打浆釜内注入打浆釜容积70%的脱盐水作为初始洗涤液,搅拌,并开启离心泵,使洗涤液经管道从收料斗的上方的喷淋装置均匀喷出;1) Inject a dispersant into the beating kettle, and the quality of the dispersant is 1.8% of the mass of the silica-alumina molecular sieve to be washed; then inject desalted water with 70% of the volume of the beating kettle into the beating kettle as the initial washing liquid, stir, and start the centrifuge Pump, so that the washing liquid is evenly sprayed from the spray device above the receiving hopper through the pipeline;

2)合成的新鲜硅铝磷分子筛浆液进入压滤机中压滤,压滤后的硅铝磷分子筛掉入收料斗,硅铝磷分子筛经喷淋的洗涤液润湿后,被双螺旋输送机输送到打浆釜中形成新混合液;2) The synthesized fresh Si-Al-P molecular sieve slurry enters the filter press for pressure filtration, and the Si-Al-P molecular sieve after pressure filtration falls into the receiving hopper. Transport to the beating tank to form a new mixed liquor;

3)压滤机压滤完新鲜的硅铝磷分子筛浆液后,打开第一阀门,调节离心泵,同时向打浆釜内连续通入脱盐水,打浆釜内的新混合液一部分经管道进入压滤机进行压滤,压滤出的液体排出压滤机,压滤出的滤饼再次进入收料斗;另一部分的新混合液经喷淋装置对收料斗内的硅铝分子筛进行润湿,润湿后的硅铝磷分子筛再次被双螺旋输送机输送到打浆釜内;进入压滤机新混合液与进入喷淋装置的新混合液的体积比为32:1;3) After the fresh silicon aluminum phosphorus molecular sieve slurry is filtered by the filter press, the first valve is opened, the centrifugal pump is adjusted, and desalted water is continuously fed into the beating kettle at the same time, and a part of the new mixed solution in the beating kettle enters the press filter through the pipeline The press filter is carried out, the liquid out of the press filter is discharged out of the filter press, and the filter cake out of the press filter enters the hopper again; the other part of the new mixed liquid is wetted by the spray device to the silicon-aluminum molecular sieve in the hopper, and the wetting The silicon-aluminum-phosphorus molecular sieve is transported to the beating kettle again by the double-screw conveyor; the volume ratio of the new mixed solution entering the filter press to the new mixed solution entering the spraying device is 32:1;

4)重复步骤2)以及步骤3)共5次当打浆釜内的溶液pH为8.0,则关闭第二阀门,停止向打浆釜通入脱盐水,同时双螺旋输送机逆向旋转,把压滤机压滤出的滤饼输送到产品罐中。4) Repeat step 2) and step 3) for a total of 5 times. When the pH of the solution in the beating kettle is 8.0, close the second valve and stop feeding desalted water into the beating kettle. The press-filtered filter cake is conveyed to the product tank.

5)打开第一阀门和第二阀门,向打浆釜内通入脱盐水,调节双螺旋输送机旋转,通过脱盐水的循环对整个装置体系进行清洗。5) Open the first valve and the second valve, pass desalted water into the beating tank, adjust the rotation of the double screw conveyor, and clean the entire device system through the circulation of desalinated water.

在整个循环洗涤时,打浆釜内的混合液中,硅铝磷分子筛的固含量在25%左右。During the whole cycle of washing, the solid content of the silicon aluminum phosphorus molecular sieve in the mixed liquid in the beating kettle is about 25%.

通入到打浆釜内的脱盐水流量始终使打浆釜内的液位保持在72%;管道的口径为72mm。The flow rate of desalted water fed into the beating kettle keeps the liquid level in the beating kettle at 72%; the diameter of the pipeline is 72mm.

压滤机单次处理的合成的新鲜硅铝磷分子筛浆液的体积为打浆釜内洗涤液体积的90%。The volume of the synthesized fresh silicon-aluminum-phosphorus molecular sieve slurry treated once by the filter press is 90% of the volume of the washing liquid in the beating kettle.

实施例一~实施例三洗涤后的催化剂的粘性物质被清除,导致物料的粘性大大降低,不再堵塞管道或设备,不经洗涤的催化剂无法进行制备丙烯,因为没有洗涤的催化剂的活性几乎为0,制备的催化剂必须要洗涤。The viscous substances of the washed catalysts in Examples 1 to 3 are removed, which greatly reduces the viscosity of the material, and no longer blocks pipelines or equipment. The unwashed catalyst cannot produce propylene, because the activity of the unwashed catalyst is almost 0, the prepared catalyst must be washed.

对比例一为只是用脱盐水洗涤的硅铝磷分子筛,共循环洗涤2次。Comparative example 1 is a silicon aluminum phosphorus molecular sieve that is only washed with desalted water, and washed twice in total.

对比例二为只是用脱盐水洗涤的硅铝磷分子筛,共循环洗涤10次。Comparative example 2 is a silicon aluminum phosphorus molecular sieve that is only washed with desalted water, and is washed 10 times in total.

将实施例一~实施例三,以及对比例一、对比例二经过洗涤后的硅铝磷分子筛同时用于乙烯、丙烯以及丁烯的制备,采用常规的实验方法,得出以下数据,The silicon-aluminum-phosphorous molecular sieves in Examples 1 to 3, and Comparative Examples 1 and 2 were used in the preparation of ethylene, propylene and butene at the same time, and the following data were obtained by using conventional experimental methods.

实验数据:Experimental data:

乙烯(选择性)Ethylene (optional) 丙烯(选择性)Propylene (optional) 丁烯(选择性)Butene (optional) 转化率Conversion rate 案例一Case number one 38.9%38.9% 40.2%40.2% 12.3%12.3% 99.78%99.78% 案例二case two 39.2%39.2% 40.0%40.0% 11.9%11.9% 99.56%99.56% 案例三case three 38.8%38.8% 41.2%41.2% 12.4%12.4% 99.49%99.49% 对比例一Comparative example one 36.2%36.2% 38.5%38.5% 14.6%14.6% 97.35%97.35% 对比例二Comparative example two 39.0%39.0% 41.9%41.9% 12.1%12.1% 99.61%99.61%

以上所述仅为本发明创造的较佳实施例而已,并不用以限制本发明创造,凡在本发明创造的精神和原则之内,所作的任何修改、等同替换、改进等,均应包含在本发明创造的保护范围之内。The above descriptions are only preferred embodiments of the present invention, and are not intended to limit the present invention. Any modifications, equivalent replacements, improvements, etc. made within the spirit and principles of the present invention shall be included in the Within the scope of protection of the present invention.

Claims (10)

1. a kind of dispersant for being used to wash sial phosphorus molecular sieve, it is characterised in that:Including according to mass ratio (0.01-0.3):1 The solution A and solution B of mixing;
The solution A include solvent, the 3-10% of solvent quality hydrochloric acid, the 0.3-0.8% of solvent quality stearmide or Stearic glyceride or the mixture of the two;The 14-32% of solvent quality glyceryl tristearate;
The solution B include solvent, the 0.01-0.03% of solvent quality formaldehyde, the 0-15% of solvent quality polyvinyl alcohol, The 0-8% of solvent quality Sodium Polyacrylate or sodium alkyl sulfonate or the mixture of the two;
The solvent of solution A is alcohol;The solvent of solution B is desalted water.
2. the dispersant according to claim 1 for being used to wash sial phosphorus molecular sieve, it is characterised in that:The alcohol is first Alcohol, ethanol, propane diols, glycerine, n-butanol, isobutanol, phenmethylol, ethylene glycol are one or two kinds of;The conductance of the desalted water It is 6.0~7.0 that rate, which is less than 5 μ S/cm, pH,.
3. the dispersant according to claim 1 or 2 for being used to wash sial phosphorus molecular sieve, it is characterised in that:The system of solution A Standby to comprise the following steps, (1) selects 30-60 DEG C of alcohol as solvent, and the 3-10% of solvent quality hydrochloric acid stirring is added in addition Uniformly;(2) stearmide or stearic glyceride or the two mixture of the addition equivalent to the 0.3-0.8% of solvent quality;(3) The glyceryl tristearate of the 14-32% equivalent to solvent quality is added, is well mixed;
The preparation of solution B comprises the following steps that (1), from desalted water as solvent, the formaldehyde that 0.01-0.03% is added in addition is stirred Mix uniform;(2) polyvinyl alcohol of the addition equivalent to the 0-15% of solvent quality;(3) addition is equivalent to the 0-8%'s of solvent quality Sodium Polyacrylate or sodium alkyl sulfonate or the mixture of the two, are well mixed.
4. a kind of device for circulating washing sial phosphorus molecular sieve, it is characterised in that:Including filter press, conveying worm and mashing Kettle;The filter press is with being beaten kettle by pipeline communication, and pipeline is provided with the first valve and centrifugal pump;The helical feed Machine is provided with recovering hopper, and the recovering hopper is located at below the outlet of filter press;Two outlets of the conveying worm connect respectively Connect products pot and mashing kettle;Spray equipment is provided with above the recovering hopper, pipe is passed through between the spray equipment and mashing kettle Road is connected, and pipeline is provided with the second valve and centrifugal pump.
5. the device of circulation washing sial phosphorus molecular sieve according to claim 4, it is characterised in that:Mashing bottom end Circulation house steward is connected with, the circulation house steward branches out two and is in charge of, connected respectively with filter press and spray equipment, and be in charge of On be respectively equipped with the first valve and the second valve;Centrifugal pump is provided with circulation house steward.
6. a kind of method that device wash cycle using as described in claim 4 or 5 washs sial phosphorus molecular sieve, its feature exists In:Comprise the following steps,
1) dispersant of the injection as described in any one of claims 1 to 3 into mashing kettle, and the quality of dispersant is silicon to be washed The 0.5-2% of aluminum molecular screen quality;Backward mashing kettle in injection mashing kettle volume 40~75% desalted water as initially washing Liquid is washed, is stirred, and opens centrifugal pump, cleaning solution is uniformly sprayed from the spray equipment of the top of recovering hopper through pipeline;
2) the fresh Si-Al molecular sieve slurries of synthesis enter press filtration in filter press, and the sial phosphorus molecular sieve after press filtration falls into rewinding Bucket, after cleaning solution wetting of the sial phosphorus molecular sieve through spray, is transported in mashing kettle by DWG and forms new mixed liquor;
3) after the complete fresh sial phosphorus molecular sieve slurries of filter press press filtration, the first valve is opened, centrifugal pump is adjusted, while to mashing The continuous new mixed liquor part being passed through in desalted water, mashing kettle enters filter press progress press filtration through pipeline in kettle, is press-filtered out Liquid discharges filter press, and the filter cake being press-filtered out is again introduced into recovering hopper;The new mixed liquor of another part is through spray equipment to rewinding Si-Al molecular sieve in bucket is soaked, and the sial phosphorus molecular sieve after wetting is transported to mashing kettle by DWG again It is interior;Volume ratio into the new mixed liquor of filter press and the new mixed liquor for entering spray equipment is (20-40):1;
4) repeat step 2) and step 3) common 2-5 times, when the pH value of solution in mashing kettle is 6.6~8.2, then close the second valve Door, stops being passed through desalted water to mashing kettle, while DWG counter-rotating, the filter cake for being press-filtered out filter press is transported to In products pot.
7. the method that use device wash cycle according to claim 6 washs sial phosphorus molecular sieve, it is characterised in that:Also Including step 5), the first valve and the second valve are opened, desalted water is passed through into mashing kettle, regulation DWG rotates, Whole device system is cleaned by the circulation of desalted water.
8. the method that use device wash cycle according to claim 6 washs sial phosphorus molecular sieve, it is characterised in that: During whole circulation washing, in the mixed liquor in mashing kettle, the solid content of sial phosphorus molecular sieve is less than 34%.
9. the method that use device wash cycle according to claim 6 washs sial phosphorus molecular sieve, it is characterised in that:It is logical Enter to the desalination water-carrying capacity in mashing kettle makes the liquid level in mashing kettle be maintained between 50~75% all the time;The bore of pipeline is 50 ~90mm.
10. the method that use device wash cycle according to claim 6 washs sial phosphorus molecular sieve, it is characterised in that: The 50- that the volume of the fresh sial phosphorus molecular sieve slurries of the synthesis of filter press single treatment is accumulated for wash liquid in mashing kettle 180%.
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109650404A (en) * 2018-12-20 2019-04-19 中国天辰工程有限公司 A kind of solid sial phosphorus molecular sieve forming method and device

Citations (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB748940A (en) * 1953-02-21 1956-05-16 Distillers Co Yeast Ltd Improvements relating to the production of resorcinol
NL151642B (en) * 1964-08-12 1976-12-15 Universal Oil Prod Co METHOD FOR OXYDERING MERCAPTANS IN A LIQUID HYDROCARBON MIXTURE AND FOR REGENERATING THE USED PHTHALOCYANINE CATALYST.
JPH01299236A (en) * 1988-05-26 1989-12-04 Mitsubishi Kasei Corp Regeneration method of palladium supported catalyst
CN1213991A (en) * 1996-01-02 1999-04-14 罗伯特E·戴维斯 Method for Improving Activity of Zeolite-Containing Granular Solid
CN1228036A (en) * 1996-06-12 1999-09-08 计划地球工业公司 Acid contacted enhanced adsorbent and/or catalyst and binder system
CN1245448A (en) * 1996-11-25 2000-02-23 戴维B·巴托里克 Method for reactivating zeolite catalysts
CN1768955A (en) * 2004-10-29 2006-05-10 中国石油化工股份有限公司 Coke Cleaning Agent and Its Application in the Regeneration Process of Coke Deactivated Catalyst
CN103173303A (en) * 2010-04-07 2013-06-26 苏扬 Regenerated cleaning agent of three-way catalytic converter
CN103203239A (en) * 2013-03-08 2013-07-17 深圳市水苑水工业技术设备有限公司 Technique and system device for regenerating exhaust gas denitration catalyst
CN103436378A (en) * 2013-08-23 2013-12-11 重庆远达催化剂制造有限公司 Cleaning solution for denitration catalyst duct blockage in thermal power plant and method for cleaning denitration catalyst by using cleaning solution
CN105344385A (en) * 2015-11-12 2016-02-24 吴亚良 High-activity catalyst regenerative liquid and preparation method thereof, and resurrection device
CN105524747A (en) * 2014-09-30 2016-04-27 惠州市祥珅实业有限公司 Cleaning agent for cleaning of three-way catalytic converter
CN106311362A (en) * 2016-08-19 2017-01-11 安徽元琛环保科技股份有限公司 Waste denitration catalyst regeneration cleaning fluid and preparation method thereof
CN106381233A (en) * 2016-08-31 2017-02-08 中国神华能源股份有限公司 Cleaning solution used for SCR catalyst, and activity recovery method of spent SCR catalyst

Patent Citations (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB748940A (en) * 1953-02-21 1956-05-16 Distillers Co Yeast Ltd Improvements relating to the production of resorcinol
NL151642B (en) * 1964-08-12 1976-12-15 Universal Oil Prod Co METHOD FOR OXYDERING MERCAPTANS IN A LIQUID HYDROCARBON MIXTURE AND FOR REGENERATING THE USED PHTHALOCYANINE CATALYST.
JPH01299236A (en) * 1988-05-26 1989-12-04 Mitsubishi Kasei Corp Regeneration method of palladium supported catalyst
CN1213991A (en) * 1996-01-02 1999-04-14 罗伯特E·戴维斯 Method for Improving Activity of Zeolite-Containing Granular Solid
CN1228036A (en) * 1996-06-12 1999-09-08 计划地球工业公司 Acid contacted enhanced adsorbent and/or catalyst and binder system
CN1245448A (en) * 1996-11-25 2000-02-23 戴维B·巴托里克 Method for reactivating zeolite catalysts
CN1768955A (en) * 2004-10-29 2006-05-10 中国石油化工股份有限公司 Coke Cleaning Agent and Its Application in the Regeneration Process of Coke Deactivated Catalyst
CN103173303A (en) * 2010-04-07 2013-06-26 苏扬 Regenerated cleaning agent of three-way catalytic converter
CN103203239A (en) * 2013-03-08 2013-07-17 深圳市水苑水工业技术设备有限公司 Technique and system device for regenerating exhaust gas denitration catalyst
CN103436378A (en) * 2013-08-23 2013-12-11 重庆远达催化剂制造有限公司 Cleaning solution for denitration catalyst duct blockage in thermal power plant and method for cleaning denitration catalyst by using cleaning solution
CN105524747A (en) * 2014-09-30 2016-04-27 惠州市祥珅实业有限公司 Cleaning agent for cleaning of three-way catalytic converter
CN105344385A (en) * 2015-11-12 2016-02-24 吴亚良 High-activity catalyst regenerative liquid and preparation method thereof, and resurrection device
CN106311362A (en) * 2016-08-19 2017-01-11 安徽元琛环保科技股份有限公司 Waste denitration catalyst regeneration cleaning fluid and preparation method thereof
CN106381233A (en) * 2016-08-31 2017-02-08 中国神华能源股份有限公司 Cleaning solution used for SCR catalyst, and activity recovery method of spent SCR catalyst

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109650404A (en) * 2018-12-20 2019-04-19 中国天辰工程有限公司 A kind of solid sial phosphorus molecular sieve forming method and device
CN109650404B (en) * 2018-12-20 2020-12-15 中国天辰工程有限公司 Method and device for forming solid silicon-aluminum-phosphorus molecular sieve

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