CN105731395A - Method for recycling purified contrast agent intermediate waste sulfuric acid - Google Patents

Method for recycling purified contrast agent intermediate waste sulfuric acid Download PDF

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Publication number
CN105731395A
CN105731395A CN201610322590.9A CN201610322590A CN105731395A CN 105731395 A CN105731395 A CN 105731395A CN 201610322590 A CN201610322590 A CN 201610322590A CN 105731395 A CN105731395 A CN 105731395A
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CN
China
Prior art keywords
contrast agent
sulfuric acid
waste sulfuric
intermediate waste
agent intermediate
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201610322590.9A
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Chinese (zh)
Inventor
刘海
叶永祥
王明波
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Wengfu Group Co Ltd
Original Assignee
Wengfu Group Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Wengfu Group Co Ltd filed Critical Wengfu Group Co Ltd
Priority to CN201610322590.9A priority Critical patent/CN105731395A/en
Publication of CN105731395A publication Critical patent/CN105731395A/en
Pending legal-status Critical Current

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Classifications

    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B17/00Sulfur; Compounds thereof
    • C01B17/69Sulfur trioxide; Sulfuric acid
    • C01B17/90Separation; Purification
    • C01B17/905Removal of organic impurities

Abstract

The invention discloses a method for recycling purified contrast agent intermediate waste sulfuric acid. Based on the physicochemical properties that a product (5-nitro dioctyl phthalate), a raw material (indirect dioctyl phthalate) and other byproducts (2,3-nitro dioctyl phthalate) of a contrast agent in waste sulfuric acid are slightly dissolved in water at normal temperature, and emulsus suspension and white crystal precipitate in the waste sulfuric acid are not dissolved in water, the method comprises the following steps: purifying by using a microfilter, recycling solid (organic matters) which is used as a raw material of a contrast agent product, and recycling liquids (mainly sulfuric acid) for calcium superphosphate production or wet-method phosphoric acid device production. The method is low in investment and operation cost and simple in operation, and meanwhile environment-friendly problems can be solved.

Description

A kind of method that contrast agent intermediate Waste Sulfuric Acid recycles after purifying
Technical field
The present invention relates to sulphuric acid, specifically a kind of contrast agent intermediate Waste Sulfuric Acid purifies, recovery and utilization technology.
Background technology
Through understanding, current contrast agent manufacturer, its intermediate Waste Sulfuric Acid uses sheet alkali to neutralize or high temperature distillation technology;Use sheet alkali to neutralize so that it is qualified discharge, not only cause contrast agent production cost high, but also waste retrieval of sulfuric acid value, cause the wasting of resources, such as deal with improperly simultaneously, cause environmental pollution.As used high temperature distillation method, after organic carbon and sulphuric acid concentration, recycling, cause contrast agent production cost high equally, investment is big, and operational risk is big.
Summary of the invention
The present invention be directed to that contrast agent intermediate Waste Sulfuric Acid processes the not enough problem existed and a kind of production cost of proposing is low, recycle costly recoverying and utilizing method.
The foregoing invention purpose of the present invention can be achieved through the following technical solutions.
A kind of method that contrast agent intermediate Waste Sulfuric Acid recycles after purifying, the method is to use pipeline or tank body discharging to enter defecator contrast agent intermediate Waste Sulfuric Acid, crystal is had to separate out (crystal is contrast agent product, raw material and by-product mixture) in view of (25 DEG C) under room temperature, use to turn to harrow and crystal is collected in cone, with being pumped into cleaning equipment, filter with the extruding of compressed air malleation, press dry, by filtrate, sulphuric acid after i.e. purifying, for compound fertilizer, general calcium or phosphoric acid plant Wet-process Phosphoric Acid Production;Run all after date, use compressed air blowback discharging, unload rear filtering residue and reclaim for contrast agent production.
Described cleaning equipment uses microporous filter, press dry two-in-one device, and pore size filter is 1-2um.
Described compressed air is 0.6Mpa.
Described contrast agent intermediate Waste Sulfuric Acid initially enters in defecator, afterwards liquid from bottom with being pumped into cleaning equipment.
nullThe principle of the present invention: produce contrast agent (5-nitro dioctyl phthalate) it is generally required to dissolve with 98% sulphuric acid and be dehydrated,After filtration,Containing indirect dioctyl phthalate in filtrate (predominantly sulphuric acid)、5-nitro dioctyl phthalate and 2、3、(its content is about 3-5%) and the nitric acid of 5-7% such as 4-nitro dioctyl phthalate,According to its organic physicochemical property,Use and filter、The equipment that press dry is by contrast agent intermediate Waste Sulfuric Acid filtration, purification,Microfilter aperture selects 1-2um(to select this bore filter speed fast,The data obtained after experiment),Adopt this method,After contrast agent intermediate Waste Sulfuric Acid purifies,In addition to being slightly soluble in water Organic substance,Other milky suspension things and crystal all filter out,Filtrate content of organics now is about: about 0.5-1%,After purification, filtrate is preferentially used for general calcium、Compound fertilizer etc.,Or 75% sulphuric acid of affluence,(75% sulphuric acid and the ratio of 98% sulphuric acid after purification) is used for phosphoric acid plant Wet-process Phosphoric Acid Production by a certain percentage,The phosphoric acid produced is for MAP、The fertilizer production such as DAP;Filtering residue reclaims the production for contrast agent.
Using this method, invest little, operating cost is low, simple to operate, and after the contrast agent intermediate Waste Sulfuric Acid of most critical is purified, filtrate and filtering residue can recycle, and reduce the production cost of contrast agent, avoid causing environmental issue simultaneously.
Accompanying drawing explanation
The process chart of Fig. 1 position present invention.
Detailed description of the invention
A kind of method that contrast agent intermediate Waste Sulfuric Acid recycles after purifying, pipeline or tank body discharging is used to enter defecator contrast agent intermediate Waste Sulfuric Acid, use to turn to harrow and crystal is collected in cone, it is delivered into cleaning equipment from bottom with pump, filter with the extruding of compressed air malleation, press dry, by filtrate, sulphuric acid after i.e. purifying, for compound fertilizer, general calcium or phosphoric acid plant Wet-process Phosphoric Acid Production;Run all after date, use compressed air blowback discharging, unload rear filtering residue and reclaim for contrast agent production.
Described cleaning equipment uses microporous filter, press dry two-in-one device, and pore size filter is 1-2um.
Described compressed air is 0.6Mpa.

Claims (4)

1. the method that a contrast agent intermediate Waste Sulfuric Acid recycles after purifying, it is characterized in that: described method is to use pipeline or tank body discharging to enter defecator contrast agent intermediate Waste Sulfuric Acid, use to turn to harrow and crystal is collected in cone, with being pumped into cleaning equipment, filter with the extruding of compressed air malleation, press dry, by filtrate, sulphuric acid after i.e. purifying, for compound fertilizer, general calcium or phosphoric acid plant Wet-process Phosphoric Acid Production;Run all after date, use compressed air blowback discharging, unload rear filtering residue and reclaim for contrast agent production.
The method that contrast agent intermediate Waste Sulfuric Acid the most according to claim 1 recycles after purifying, it is characterised in that: described cleaning equipment uses microporous filter, press dry two-in-one device, and pore size filter is 1-2um.
The method that contrast agent intermediate Waste Sulfuric Acid the most according to claim 1 recycles after purifying, it is characterised in that: described compressed air is 0.6Mpa.
Contrast agent intermediate Waste Sulfuric Acid the most according to claim 1 purify after recycle method, it is characterised in that: described contrast agent intermediate Waste Sulfuric Acid initially enters in defecator, afterwards liquid from bottom with being pumped into cleaning equipment.
CN201610322590.9A 2016-05-16 2016-05-16 Method for recycling purified contrast agent intermediate waste sulfuric acid Pending CN105731395A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201610322590.9A CN105731395A (en) 2016-05-16 2016-05-16 Method for recycling purified contrast agent intermediate waste sulfuric acid

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201610322590.9A CN105731395A (en) 2016-05-16 2016-05-16 Method for recycling purified contrast agent intermediate waste sulfuric acid

Publications (1)

Publication Number Publication Date
CN105731395A true CN105731395A (en) 2016-07-06

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Family Applications (1)

Application Number Title Priority Date Filing Date
CN201610322590.9A Pending CN105731395A (en) 2016-05-16 2016-05-16 Method for recycling purified contrast agent intermediate waste sulfuric acid

Country Status (1)

Country Link
CN (1) CN105731395A (en)

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1986390A (en) * 2006-12-26 2007-06-27 四川泸天化股份有限公司 Process of purifying and recovering waste sulfuric acid containing organic impurity
CN102010082A (en) * 2010-09-29 2011-04-13 南京梅山冶金发展有限公司 Treatment method for recycling waste dilute sulfuric acid
CN102897720A (en) * 2012-10-11 2013-01-30 瓮福(集团)有限责任公司 Recycling method of waste diluted sulfuric acid in sulfuric acid device
CN102951627A (en) * 2012-10-18 2013-03-06 陕西比迪欧化工有限公司 System and method for recycling and utilizing waste sulfuric acid

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1986390A (en) * 2006-12-26 2007-06-27 四川泸天化股份有限公司 Process of purifying and recovering waste sulfuric acid containing organic impurity
CN102010082A (en) * 2010-09-29 2011-04-13 南京梅山冶金发展有限公司 Treatment method for recycling waste dilute sulfuric acid
CN102897720A (en) * 2012-10-11 2013-01-30 瓮福(集团)有限责任公司 Recycling method of waste diluted sulfuric acid in sulfuric acid device
CN102951627A (en) * 2012-10-18 2013-03-06 陕西比迪欧化工有限公司 System and method for recycling and utilizing waste sulfuric acid

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Application publication date: 20160706