CN112973631B - Preparation method of activated carbon filter element for filtering total organic carbon in electroplating solution - Google Patents

Preparation method of activated carbon filter element for filtering total organic carbon in electroplating solution Download PDF

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CN112973631B
CN112973631B CN202110192908.7A CN202110192908A CN112973631B CN 112973631 B CN112973631 B CN 112973631B CN 202110192908 A CN202110192908 A CN 202110192908A CN 112973631 B CN112973631 B CN 112973631B
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activated carbon
filter element
carbon fiber
total organic
filtering
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CN112973631A (en
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李凤丸
黄勇
杜玉
吴雯燊
刘帆
韩娇娇
徐麟
杨代军
李刚
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Shanghai Elo Technology Co ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/20Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D15/00Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
    • B01D15/08Selective adsorption, e.g. chromatography
    • B01D15/10Selective adsorption, e.g. chromatography characterised by constructional or operational features
    • B01D15/20Selective adsorption, e.g. chromatography characterised by constructional or operational features relating to the conditioning of the sorbent material
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D21/00Processes for servicing or operating cells for electrolytic coating

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Analytical Chemistry (AREA)
  • Electrochemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Inorganic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Chemical Or Physical Treatment Of Fibers (AREA)
  • Electroplating Methods And Accessories (AREA)
  • Water Treatment By Sorption (AREA)
  • Filtering Materials (AREA)

Abstract

The invention provides a preparation method of an activated carbon filter element for filtering total organic carbon in electroplating solution, which comprises the following steps: taking the carbon powder for later use; carrying out peroxidation treatment on the activated carbon fiber to obtain oxidized activated carbon fiber; taking carbon powder and oxidized activated carbon fiber, adding an adhesive, and stirring to obtain activated carbon fiber adhered with the carbon powder; winding activated carbon fiber stuck with carbon powder on a porous plastic pipe pre-wrapped with non-woven fabric, wrapping the non-woven fabric again when the thickness reaches 15mm, and drying to obtain a finished product of the activated carbon filter core; then the filter element is placed into the filter element body to prepare the active carbon filter element for filtering the total organic carbon in the electroplating solution. The preparation method of the activated carbon filter element for filtering the total organic carbon in the electroplating solution can filter the total organic carbon in the electroplating solution on line, improve the stability of the electroplating bath solution, prolong the service life of the bath solution and the reliability of a plated part to the maximum extent, reduce the cost and protect the environment.

Description

Preparation method of activated carbon filter element for filtering total organic carbon in electroplating solution
Technical Field
The invention belongs to the field of electroplating, and particularly relates to a preparation method of an activated carbon filter element for filtering total organic carbon in electroplating solution.
Background
Various products such as carbon powder, carbon particles, carbon filter elements, carbon fiber filter elements and the like applied to the market at present are mainly used for water purification treatment, so that the effects of deodorization, decoloration and sterilization are achieved, and heavy metal, organic molecules or ions and substances which are difficult to degrade are adsorbed in the wastewater treatment; although the method for filtering and adsorbing impurities is widely applied, no product or method with outstanding targeted effect is found in the electroplating industry at present.
Electroplating is a process of plating a thin layer of other metals or alloys on the surface of some metals by using the principle of electrolysis, and is a process of attaching a layer of metal film on the surface of a metal or other material product by using the action of electrolysis so as to prevent the oxidation (such as corrosion) of the metal, improve the wear resistance, the conductivity, the light reflection property, the corrosion resistance, the beauty and the like. In the electroplating process, besides the main salt for providing metal ions, a buffer for stabilizing the solution, a brightener for increasing the brightness of the plated piece, a grain refiner, a leveling agent, a wetting agent and other special additives are usually added. All these auxiliary substances are collectively called additives, and the compositions of the additives are different according to the purpose and requirement of electroplating.
These additives are macromolecular organic substances, mainly including: hydroxyethyl cellulose (HEC), sodium 3-mercapto-1-propanesulfonate (MPS), polyethylene glycol (PEG), sodium polydithio-dipropyl sulfonate (SPS), Polyethyleneimine (PEI), hydrolyzed collagen, and the like, wherein the molecular weight of the additives is different from thousands to tens of thousands. During the electroplating process, the macromolecular organic matters are gradually cracked to form micromolecular byproducts which are continuously accumulated in the bath solution along with the increase of the production time. Generally, a small portion of the byproducts accumulated in the bath solution will be carried away by the plated parts, but a large portion will remain in the bath solution, and the common operation method is to continuously dilute or directly replace the bath before the bath solution is as long as the bath solution is available.
Disclosure of Invention
It is an object of the present invention to provide a method of making an activated carbon filter cartridge for filtering total organic carbon in electroplating baths and to provide at least the advantages described hereinafter.
The invention also aims to provide a preparation method of the activated carbon filter element for filtering the total organic carbon in the electroplating solution, which can filter the total organic carbon in the electroplating solution on line, improve the stability of the electroplating bath solution, prolong the service life of the bath solution and improve the reliability of a plated part to the utmost extent, reduce the cost and protect the environment.
The technical scheme of the invention is as follows:
the preparation method of the activated carbon filter element for filtering the total organic carbon in the electroplating solution comprises the following steps:
taking carbon powder for standby, wherein the small pore radius of the carbon powder is 1-3nm, the transition pore radius is 2-100nm, the large pore radius is 100-100000nm, and the specific surface area is 1500 square meters per gram;
taking activated carbon fibers for standby, wherein the pore diameter of the activated carbon fibers is 0.5-1.5nm, the specific surface area is 1500 square meters per gram, and the activated carbon fibers are subjected to peroxidation treatment to obtain oxidized activated carbon fibers;
taking the carbon powder and the oxidized activated carbon fiber in a weight ratio of 4:6, adding an adhesive, and stirring for at least 30min to obtain the activated carbon fiber adhered with the carbon powder;
winding activated carbon fiber stuck with carbon powder on a porous plastic pipe pre-wrapped with non-woven fabric, and wrapping the non-woven fabric again when the thickness of the activated carbon fiber stuck with the carbon powder reaches 15mm to obtain a semi-finished product of the activated carbon filter core inner core;
drying the semi-finished product of the inner core of the activated carbon filter core for 4 hours at the temperature of 110-125 ℃ to obtain a finished product of the inner core of the activated carbon filter core;
and then putting the finished product of the inner core of the activated carbon filter element into the filter element body to prepare the activated carbon filter element for filtering the total organic carbon in the electroplating solution.
Preferably, in the method for preparing an activated carbon filter element for filtering total organic carbon in electroplating solution, subjecting the activated carbon fiber to an oxidation treatment includes:
mixing the activated carbon fiber and persulfate according to the weight ratio of 9:0.7, carrying out oxidation reaction for 1-4min at the temperature of 62-67 ℃, then cooling to 34-36 ℃, adding sodium peroxide with the weight being 0.08 time of that of the activated carbon fiber, heating to 73-75 ℃, carrying out oxidation reaction for 3-5min again, and cooling to room temperature to obtain the oxidized activated carbon fiber.
Preferably, in the preparation method of the activated carbon filter element for filtering the total organic carbon in the electroplating solution, the activated carbon fibers comprise two types, and the lengths of the two types are respectively 50-70mm and 200-400 mm.
Preferably, in the preparation method of the activated carbon filter core for filtering the total organic carbon in the electroplating solution, when the thickness of the activated carbon fiber adhered with the carbon powder reaches 4mm, 8mm and 12mm, a layer of activated carbon fiber felt with the thickness of 1mm, 2mm and 1mm is respectively adhered on the surface.
The invention has the following beneficial effects:
after the activated carbon fiber is subjected to peroxidation treatment, the content of oxygen-containing functional groups on the surface is increased, the polarity of the surface is enhanced, and the adsorption performance is improved;
the carbon powder is adhered to the activated carbon fiber, so that the specific surface area of the activated carbon fiber is increased, and the adsorbability of the activated carbon fiber is further enhanced.
Additional advantages, objects, and features of the invention will be set forth in part in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention.
Detailed Description
The present invention is described in further detail below to enable those skilled in the art to practice the invention with reference to the description.
It will be understood that terms such as "having," "including," and "comprising," as used herein, do not preclude the presence or addition of one or more other elements or groups thereof.
The invention provides a preparation method of an activated carbon filter element for filtering total organic carbon in electroplating solution, which comprises the following steps:
taking carbon powder for standby, wherein the small pore radius of the carbon powder is 1-3nm, the transition pore radius is 2-100nm, the large pore radius is 100-100000nm, and the specific surface area is 1500 square meters per gram;
taking activated carbon fibers for standby, wherein the pore diameter of the activated carbon fibers is 0.5-1.5nm, the specific surface area is 1500 square meters per gram, and the activated carbon fibers are subjected to peroxidation treatment to obtain oxidized activated carbon fibers;
taking carbon powder and oxidized activated carbon fiber in a weight ratio of 4:6, adding an adhesive, and stirring for at least 30min to obtain activated carbon fiber adhered with the carbon powder;
winding activated carbon fiber stuck with carbon powder on a porous plastic pipe pre-wrapped with non-woven fabric, and wrapping the non-woven fabric again when the thickness of the activated carbon fiber stuck with the carbon powder reaches 15mm to obtain a semi-finished product of the activated carbon filter core inner core;
drying the semi-finished product of the inner core of the activated carbon filter core for 4 hours at the temperature of 110-125 ℃ to obtain a finished product of the inner core of the activated carbon filter core;
and then putting the finished product of the inner core of the activated carbon filter element into the filter element body to prepare the activated carbon filter element for filtering the total organic carbon in the electroplating solution.
The non-woven fabric can prevent loss of the carbon powder, avoid pollution of the carbon powder to electroplating liquid and ensure that the adsorbability of the non-woven fabric is not reduced.
The invention relates to the activated carbon part only, and other parts of the filter element can be selected by a person skilled in the art according to actual conditions without detailed description.
In one embodiment of the method for preparing an activated carbon filter element for filtering total organic carbon in electroplating solution, the step of subjecting the activated carbon fiber to oxidation treatment includes:
mixing activated carbon fiber and persulfate according to the weight ratio of 9:0.7, then carrying out oxidation reaction for 1-4min at the temperature of 62-67 ℃, then cooling to 34-36 ℃, adding sodium peroxide with the weight being 0.08 times of that of the activated carbon fiber, heating to 73-75 ℃, then carrying out oxidation reaction for 3-5min again, and cooling to room temperature to obtain oxidized activated carbon fiber;
after two times of oxidation reaction, the number of oxygen-containing functional groups is further increased, and macromolecular organic matters in the electroplating solution can be adsorbed more.
In an embodiment of the preparation method of the activated carbon filter element for filtering total organic carbon in the electroplating solution provided by the invention, the activated carbon fibers comprise two types, the lengths of the two types are respectively 50-70mm and 200-400mm, and the activated carbon fibers with different lengths can be wound into a lump and bonded with carbon powder more fully and thoroughly.
In an embodiment of the method for preparing the activated carbon filter element for filtering the total organic carbon in the electroplating solution, when the thickness of the activated carbon fiber adhered with the carbon powder reaches 4mm, 8mm and 12mm, a layer of activated carbon fiber felt with the thickness of 1mm, 2mm and 1mm is respectively adhered on the surface, so that the activated carbon fiber can be protected, and the adsorption effect can be improved.
Taking the electroplating and tinning treatment liquid as an example, the total organic carbon content in the electroplating treatment liquid is 1500ppm, the total organic carbon content after the treatment of the original filter is 338ppm, the total organic carbon content is reduced to 224ppm after the activated carbon filter element provided by the invention is installed for filtering for 6 hours, the total organic carbon content is reduced to 107ppm after two filters are installed for filtering for 6 hours, the national emission standard is 300ppm, and the adsorption effect is obvious.
According to the preparation method of the activated carbon filter element for filtering the total organic carbon in the electroplating solution, the prepared filter element can be directly placed in a filter for filtering, and the electroplating solution can be surface electroplating treatment liquid medicine such as tinning, coppering, nickeling, gilding and the like;
according to the preparation method of the activated carbon filter element for filtering the total organic carbon in the electroplating solution, the treatment time of the prepared filter element is more than 6 hours, and the filter element can effectively adsorb macromolecular organic matters and redox substances cracked in the electroplating additive;
the total organic carbon content (TOC) of the electroplating bath solution before and after the detection treatment is used for confirming the specific adsorption capacity, and the number of the filter elements can be increased for carrying out multiple times of filtration so as to ensure that the total organic carbon content therein meets the requirement.
While embodiments of the invention have been disclosed above, it is not intended to be limited to the details shown in the description and the examples, which are set forth, but are fully applicable to various fields of endeavor as are suited to the particular use contemplated, and further modifications will readily occur to those skilled in the art, since the invention is not limited to the details shown and described without departing from the general concept as defined by the appended claims and their equivalents.

Claims (1)

1. The preparation method of the active carbon filter element for filtering the total organic carbon in the electroplating solution is characterized by comprising the following steps:
taking carbon powder for standby, wherein the small pore radius of the carbon powder is 1-3nm, the transition pore radius is 2-100nm, the large pore radius is 100-100000nm, and the specific surface area is 1500 square meters per gram;
taking activated carbon fibers for standby, wherein the pore diameter of the activated carbon fibers is 0.5-1.5nm, the specific surface area is 1500 square meters per gram, and the activated carbon fibers are subjected to peroxidation treatment to obtain oxidized activated carbon fibers;
taking carbon powder and oxidized activated carbon fiber in a weight ratio of 4:6, adding an adhesive, and stirring for at least 30min to obtain activated carbon fiber adhered with the carbon powder;
winding activated carbon fiber stuck with carbon powder on a porous plastic pipe pre-wrapped with non-woven fabric, and wrapping the non-woven fabric again when the thickness of the activated carbon fiber stuck with the carbon powder reaches 15mm to obtain a semi-finished product of the activated carbon filter core inner core;
drying the semi-finished product of the inner core of the activated carbon filter core for 4 hours at the temperature of 110-125 ℃ to obtain a finished product of the inner core of the activated carbon filter core;
then putting the finished product of the activated carbon filter element inner core into the filter element body to prepare the activated carbon filter element for filtering the total organic carbon in the electroplating solution; wherein;
subjecting the activated carbon fiber to a peroxidation treatment comprises:
mixing activated carbon fiber and persulfate according to the weight ratio of 9:0.7, then carrying out oxidation reaction for 1-4min at the temperature of 62-67 ℃, then cooling to 34-36 ℃, adding sodium peroxide with the weight being 0.08 times of that of the activated carbon fiber, heating to 73-75 ℃, then carrying out oxidation reaction for 3-5min again, and cooling to room temperature to obtain oxidized activated carbon fiber;
the activated carbon fibers comprise two types, and the lengths of the two types are respectively 50-70mm and 200-400 mm;
when the thickness of the activated carbon fiber stuck with the carbon powder reaches 4mm, 8mm and 12mm, respectively sticking a layer of activated carbon fiber felt with the thickness of 1mm, 2mm and 1mm on the surface.
CN202110192908.7A 2021-02-20 2021-02-20 Preparation method of activated carbon filter element for filtering total organic carbon in electroplating solution Active CN112973631B (en)

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JP2002362915A (en) * 2001-06-11 2002-12-18 Showa Denko Kk Carbon material and manufacturing method thereof and application thereof
CN103397404B (en) * 2013-07-15 2015-05-13 北京林业大学 Method for increasing specific surface area of wooden active carbon fiber
CN105084572B (en) * 2015-09-14 2018-02-13 广东正业科技股份有限公司 A kind of activated carbon fibrous composite and preparation method thereof and a kind of active carbon fabric composite filter element
CN109261137A (en) * 2018-09-30 2019-01-25 江苏斯沃得环保科技有限公司 A kind of composite reactive Carbon Materials and preparation method
CN111302342B (en) * 2020-03-23 2022-12-23 江苏科净炭纤维有限公司 Process for manufacturing super-filtration module by using activated carbon fiber powder and carbonization and activation device

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