CN107096503A - It is a kind of to be used for the Pd Me HMS molecular sieve preparation methods of the metal impurities in cup in adsorption cleaning running water - Google Patents

It is a kind of to be used for the Pd Me HMS molecular sieve preparation methods of the metal impurities in cup in adsorption cleaning running water Download PDF

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CN107096503A
CN107096503A CN201710301014.0A CN201710301014A CN107096503A CN 107096503 A CN107096503 A CN 107096503A CN 201710301014 A CN201710301014 A CN 201710301014A CN 107096503 A CN107096503 A CN 107096503A
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solution
molecular sieves
oil bath
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hms
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刘志伟
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Changle Net Able New Mstar Technology 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
    • B01J20/0203Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
    • B01J20/0225Compounds of Fe, Ru, Os, Co, Rh, Ir, Ni, Pd, Pt
    • 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
    • B01J20/0203Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
    • B01J20/0274Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04 characterised by the type of anion
    • B01J20/0296Nitrates of compounds other than those provided for in B01J20/04
    • 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
    • B01J20/22Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
    • B01J20/223Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material containing metals, e.g. organo-metallic compounds, coordination complexes
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/28Treatment of water, waste water, or sewage by sorption
    • C02F1/285Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/10Inorganic compounds
    • C02F2101/20Heavy metals or heavy metal compounds

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  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
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Abstract

It is used for the Pd Me HMS molecular sieve preparation methods of the metal impurities in cup in adsorption cleaning running water the invention discloses a kind of, respectively with hexadecylamine (HDA), MTMS (MTMOS), palladium nitrate, isopropanol, tetraethyl orthosilicate (TEOS) ethanol, the raw material such as ammonium chloride water is by magnetization, and the Pd Me HMS molecular sieves that the modified method such as ultrasonic oscillation is prepared are used for metal impurities in cup in adsorption cleaning running water and other effects very well.

Description

It is a kind of to be used for the Pd-Me-HMS of the metal impurities in cup in adsorption cleaning running water Molecular sieve preparation method
Technical field
It is used for the Pd-Me-HMS system with molecular sieve for preparing of the metal impurities in cup in adsorption cleaning running water the present invention relates to a kind of Preparation Method, belongs to adsorption technology field.
Background technology
Water is Source of life.The water quality of drinking water has material impact to body health.It is increasingly tight due to pollution of waterhead The drinking water species that running water is further processed for weight, the quality of fears are entertained that running water and selecting.At present in some Europe Developed country of U.S., most of families are drinking purified water or pure water;In China, the user of purified water and pure water is also year by year Increase sharply.But some water purifier effects are not fine, a kind of Pd-Me-HMS molecular sieves of modification of the invention are used for cup In good effect is achieved to purified water.
The content of the invention
In view of the above-mentioned problems of the prior art, the present invention provides a kind of be used in cup in adsorption cleaning running water The Pd-Me-HMS molecular sieve preparation methods of metal impurities, absorption purifying effect is fine.
To achieve these goals, the technical solution adopted by the present invention is:One kind is used for adsorption cleaning running water in cup In metal impurities Pd-Me-HMS molecular sieve preparation methods, comprise the following steps:
Step 1,100 DEG C of oil bath ultrasound 3h removal of impurities under ultrasonic oscillation by hexadecylamine (HDA) and ethanol first;
Solution A is formed in step 2, the solution for being made up of hexadecylamine (HDA) addition deionized water and ethanol, magnetic force is stirred Mix 100 DEG C of oil bath ultrasound 3h;
Step 3, by MTMS (MTMOS), palladium nitrate, isopropanol, tetraethyl orthosilicate (TEOS) is in ultrasound Ripple shakes 100 DEG C of 2h removal of impurities of oil bath;
Step 4, by MTMS (MTMOS), palladium nitrate is added to by isopropanol and tetraethyl orthosilicate (TEOS) solution B, 100 DEG C of oil bath 2h of magnetic agitation are formed in the mixed solution of composition;
Step 5, solution A mixed with solution B, 100 DEG C of oil bath 4h of magnetic agitation;
Step 6, by above-mentioned mixed solution with microwave treatment 2h be modified;
Step 7, using flame spraying one-step synthesis Pd-Me-HMS molecular sieves, i.e., above-mentioned solution is added to flame spray In the needle tubing of injection device, then add the CH4 of high heating value, and be passed through oxygen, while igniting by obtained solution from pin hole with The form of ion ejects the rapid synthesis Pd-Me-HMS molecular sieves at 3000 DEG C;
Step 8 and then the centrifugation under centrifugal separator, are dried, and are finally forged in Muffle furnace under sufficient air atmosphere 6h is burnt, Pd-Me-HMS molecular sieves are obtained;
Step 9, by obtained Pd-Me-HMS molecular sieves under sampling machine sample preparation into 30-60 mesh;
Step 10, obtained Pd-Me-HMS molecular sieves are urged by inlaying attachment method and be embedded on cup inwall, with stainless The granular Pd-Me-HMS molecular sieves of wire perforation, are then woven in the centre of lautertuns above cup.
Beneficial effect:Pd-Me-HMS molecular sieves of the present invention are used to have in good adsorption cleaning running water in cup Metal ion, impurity and other effects, the present invention changes the skeleton of molecular sieve, enhances suction-operated by introducing Pd elements. By magnetic agitation in preparation process, ultrasonic oscillation, flame spraying synthesis, these method of modifying of microwave treatment make obtained Molecular sieve adsorption purifies the metal ion in running water, and impurity and other effects is greatly promoted, wherein palladium nitrate, methyl trimethoxy epoxide silicon Alkane (MTMOS) mass ratio 1:9,0.5g palladium nitrates, 4.5g MTMSs (MTMOS), 10ml ethanol, the positive silicic acid of 5ml Ethyl ester, 8g hexadecylamines (HDA), 6g isopropanols, 200ml deionized waters, palladium nitrate, MTMS (MTMOS) matter Amount compares 1:10 sample, 0.5g palladium nitrates, 4.5g MTMSs (MTMOS), 10ml ethanol, 5ml tetraethyl orthosilicates, 8g Hexadecylamine (HDA), 6g isopropanols, Pd-Me-HMS molecular sieves made from 200ml deionized waters are used for adsorption cleaning water in cup Effect is best.
Embodiment
Embodiment 1 produces palladium nitrate, MTMS (MTMOS) mass ratio 1:1 sample.0.5g palladium nitrates, 0.5g MTMSs (MTMOS), 10ml ethanol, 5ml tetraethyl orthosilicates, 8g hexadecylamines (HDA), 6g isopropanols, 200ml deionized waters.
Step 1, by 8g hexadecylamines (HDA) and 10ml ethanol, 100 DEG C of oil bath ultrasound 3h are removed under ultrasonic oscillation first It is miscellaneous;
Formed in step 2, the solution for being made up of 8g hexadecylamines (HDA) addition 200ml deionized waters and 10ml ethanol Solution A, 100 DEG C of oil bath ultrasound 3h of magnetic agitation;
Step 3, by MTMS (MTMOS), palladium nitrate, isopropanol, tetraethyl orthosilicate (TEOS) is in ultrasound Ripple shakes 100 DEG C of 2h removal of impurities of oil bath;
Step 4, by 0.5g MTMSs (MTMOS), 0.5g palladium nitrates are added to by 6g isopropanols and 5ml Solution B, 100 DEG C of oil bath 2h of magnetic agitation are formed in the mixed solution of tetraethyl orthosilicate (TEOS) composition;
Step 5, solution A mixed with solution B, 100 DEG C of oil bath 4h of magnetic agitation;
Step 6, by above-mentioned mixed solution with microwave treatment 2h be modified;
Step 7, using flame spraying one-step synthesis Pd-Me-HMS molecular sieves, i.e., above-mentioned solution is added to flame spray In the needle tubing of injection device, then add the CH4 of high heating value, and be passed through oxygen, while igniting by obtained solution from pin hole with The form of ion ejects the rapid synthesis Pd-Me-HMS molecular sieves at 3000 DEG C;
Step 8 and then the centrifugation under centrifugal separator, are dried, and are finally forged in Muffle furnace under sufficient air atmosphere 6h is burnt, Pd-Me-HMS molecular sieves are obtained;
Step 9, by obtained Pd-Me-HMS molecular sieves under sampling machine sample preparation into 30-60 mesh;
Step 10, obtained Pd-Me-HMS molecular sieves are urged by inlaying attachment method and be embedded on cup inwall, with stainless The granular Pd-Me-HMS molecular sieves of wire perforation, are then woven in the centre of lautertuns above cup.
Embodiment 2 produces palladium nitrate, MTMS (MTMOS) mass ratio 1:2 sample.0.5g palladium nitrates, 1g MTMS (MTMOS), 10ml ethanol, 5ml tetraethyl orthosilicates, 8g hexadecylamines (HDA), 6g isopropanols, 200ml Deionized water.
Step 1, by 8g hexadecylamines (HDA) and 10ml ethanol, 100 DEG C of oil bath ultrasound 3h are removed under ultrasonic oscillation first It is miscellaneous;
Formed in step 2, the solution for being made up of 8g hexadecylamines (HDA) addition 200ml deionized waters and 10ml ethanol Solution A, 100 DEG C of oil bath ultrasound 3h of magnetic agitation;
Step 3, by MTMS (MTMOS), palladium nitrate, isopropanol, tetraethyl orthosilicate (TEOS) is in ultrasound Ripple shakes 100 DEG C of 2h removal of impurities of oil bath;
Step 4, by 1g MTMSs (MTMOS), 0.5g palladium nitrates are added to by 6g isopropanols and 5ml just Solution B, 100 DEG C of oil bath 2h of magnetic agitation are formed in the mixed solution of silester (TEOS) composition;
Step 5, solution A mixed with solution B, 100 DEG C of oil bath 4h of magnetic agitation;
Step 6, by above-mentioned mixed solution with microwave treatment 2h be modified;
Step 7, using flame spraying one-step synthesis Pd-Me-HMS molecular sieves, i.e., above-mentioned solution is added to flame spray In the needle tubing of injection device, then add the CH4 of high heating value, and be passed through oxygen, while igniting by obtained solution from pin hole with The form of ion ejects the rapid synthesis Pd-Me-HMS molecular sieves at 3000 DEG C;
Step 8 and then the centrifugation under centrifugal separator, are dried, and are finally forged in Muffle furnace under sufficient air atmosphere 6h is burnt, Pd-Me-HMS molecular sieves are obtained;
Step 9, by obtained Pd-Me-HMS molecular sieves under sampling machine sample preparation into 30-60 mesh;
Step 10, obtained Pd-Me-HMS molecular sieves are urged by inlaying attachment method and be embedded on cup inwall, with stainless The granular Pd-Me-HMS molecular sieves of wire perforation, are then woven in the centre of lautertuns above cup.
Embodiment 3 produces palladium nitrate, MTMS (MTMOS) mass ratio 1:3 sample.0.5g palladium nitrates, 1.5g MTMSs (MTMOS), 10ml ethanol, 5ml tetraethyl orthosilicates, 8g hexadecylamines (HDA), 6g isopropanols, 200ml deionized waters.
Step 1, by 8g hexadecylamines (HDA) and 10ml ethanol, 100 DEG C of oil bath ultrasound 3h are removed under ultrasonic oscillation first It is miscellaneous;
Formed in step 2, the solution for being made up of 8g hexadecylamines (HDA) addition 200ml deionized waters and 10ml ethanol Solution A, 100 DEG C of oil bath ultrasound 3h of magnetic agitation;
Step 3, by MTMS (MTMOS), palladium nitrate, isopropanol, tetraethyl orthosilicate (TEOS) is in ultrasound Ripple shakes 100 DEG C of 2h removal of impurities of oil bath;
Step 4, by 1.5g MTMSs (MTMOS), 0.5g palladium nitrates are added to by 6g isopropanols and 5ml Solution B, 100 DEG C of oil bath 2h of magnetic agitation are formed in the mixed solution of tetraethyl orthosilicate (TEOS) composition;
Step 5, solution A mixed with solution B, 100 DEG C of oil bath 4h of magnetic agitation;
Step 6, by above-mentioned mixed solution with microwave treatment 2h be modified;
Step 7, using flame spraying one-step synthesis Pd-Me-HMS molecular sieves, i.e., above-mentioned solution is added to flame spray In the needle tubing of injection device, then add the CH4 of high heating value, and be passed through oxygen, while igniting by obtained solution from pin hole with The form of ion ejects the rapid synthesis Pd-Me-HMS molecular sieves at 3000 DEG C;
Step 8 and then the centrifugation under centrifugal separator, are dried, and are finally forged in Muffle furnace under sufficient air atmosphere 6h is burnt, Pd-Me-HMS molecular sieves are obtained;
Step 9, by obtained Pd-Me-HMS molecular sieves under sampling machine sample preparation into 30-60 mesh;
Step 10, obtained Pd-Me-HMS molecular sieves are urged by inlaying attachment method and be embedded on cup inwall, with stainless The granular Pd-Me-HMS molecular sieves of wire perforation, are then woven in the centre of lautertuns above cup.
Embodiment 4 produces palladium nitrate, MTMS (MTMOS) mass ratio 1:4 sample.0.5g palladium nitrates, 2g MTMS (MTMOS), 10ml ethanol, 5ml tetraethyl orthosilicates, 8g hexadecylamines (HDA), 6g isopropanols, 200ml Deionized water.
Step 1, by 8g hexadecylamines (HDA) and 10ml ethanol, 100 DEG C of oil bath ultrasound 3h are removed under ultrasonic oscillation first It is miscellaneous;
Formed in step 2, the solution for being made up of 8g hexadecylamines (HDA) addition 200ml deionized waters and 10ml ethanol Solution A, 100 DEG C of oil bath ultrasound 3h of magnetic agitation;
Step 3, by MTMS (MTMOS), palladium nitrate, isopropanol, tetraethyl orthosilicate (TEOS) is in ultrasound Ripple shakes 100 DEG C of 2h removal of impurities of oil bath;
Step 4, by 2g MTMSs (MTMOS), 0.5g palladium nitrates are added to by 6g isopropanols and 5ml just Solution B, 100 DEG C of oil bath 2h of magnetic agitation are formed in the mixed solution of silester (TEOS) composition;
Step 5, solution A mixed with solution B, 100 DEG C of oil bath 4h of magnetic agitation;
Step 6, by above-mentioned mixed solution with microwave treatment 2h be modified;
Step 7, using flame spraying one-step synthesis Pd-Me-HMS molecular sieves, i.e., above-mentioned solution is added to flame spray In the needle tubing of injection device, then add the CH4 of high heating value, and be passed through oxygen, while igniting by obtained solution from pin hole with The form of ion ejects the rapid synthesis Pd-Me-HMS molecular sieves at 3000 DEG C;
Step 8 and then the centrifugation under centrifugal separator, are dried, and are finally forged in Muffle furnace under sufficient air atmosphere 6h is burnt, Pd-Me-HMS molecular sieves are obtained;
Step 9, by obtained Pd-Me-HMS molecular sieves under sampling machine sample preparation into 30-60 mesh;
Step 10, obtained Pd-Me-HMS molecular sieves are urged by inlaying attachment method and be embedded on cup inwall, with stainless The granular Pd-Me-HMS molecular sieves of wire perforation, are then woven in the centre of lautertuns above cup.
Embodiment 5 produces palladium nitrate, MTMS (MTMOS) mass ratio 1:5 sample.0.5g palladium nitrates, 2.5g MTMSs (MTMOS), 10ml ethanol, 5ml tetraethyl orthosilicates, 8g hexadecylamines (HDA), 6g isopropanols, 200ml deionized waters.
Step 1, by 8g hexadecylamines (HDA) and 10ml ethanol, 100 DEG C of oil bath ultrasound 3h are removed under ultrasonic oscillation first It is miscellaneous;
Formed in step 2, the solution for being made up of 8g hexadecylamines (HDA) addition 200ml deionized waters and 10ml ethanol Solution A, 100 DEG C of oil bath ultrasound 3h of magnetic agitation;
Step 3, by MTMS (MTMOS), palladium nitrate, isopropanol, tetraethyl orthosilicate (TEOS) is in ultrasound Ripple shakes 100 DEG C of 2h removal of impurities of oil bath;
Step 4, by 2.5g MTMSs (MTMOS), 0.5g palladium nitrates are added to by 6g isopropanols and 5ml Solution B, 100 DEG C of oil bath 2h of magnetic agitation are formed in the mixed solution of tetraethyl orthosilicate (TEOS) composition;
Step 5, solution A mixed with solution B, 100 DEG C of oil bath 4h of magnetic agitation;
Step 6, by above-mentioned mixed solution with microwave treatment 2h be modified;
Step 7, using flame spraying one-step synthesis Pd-Me-HMS molecular sieves, i.e., above-mentioned solution is added to flame spray In the needle tubing of injection device, then add the CH4 of high heating value, and be passed through oxygen, while igniting by obtained solution from pin hole with The form of ion ejects the rapid synthesis Pd-Me-HMS molecular sieves at 3000 DEG C;
Step 8 and then the centrifugation under centrifugal separator, are dried, and are finally forged in Muffle furnace under sufficient air atmosphere 6h is burnt, Pd-Me-HMS molecular sieves are obtained;
Step 9, by obtained Pd-Me-HMS molecular sieves under sampling machine sample preparation into 30-60 mesh;
Step 10, obtained Pd-Me-HMS molecular sieves are urged by inlaying attachment method and be embedded on cup inwall, with stainless The granular Pd-Me-HMS molecular sieves of wire perforation, are then woven in the centre of lautertuns above cup.
Embodiment 6 produces palladium nitrate, MTMS (MTMOS) mass ratio 1:6 sample.0.5g palladium nitrates, 3g MTMS (MTMOS), 10ml ethanol, 5ml tetraethyl orthosilicates, 8g hexadecylamines (HDA), 6g isopropanols, 200ml Deionized water.
Step 1, by 8g hexadecylamines (HDA) and 10ml ethanol, 100 DEG C of oil bath ultrasound 3h are removed under ultrasonic oscillation first It is miscellaneous;
Formed in step 2, the solution for being made up of 8g hexadecylamines (HDA) addition 200ml deionized waters and 10ml ethanol Solution A, 100 DEG C of oil bath ultrasound 3h of magnetic agitation;
Step 3, by MTMS (MTMOS), palladium nitrate, isopropanol, tetraethyl orthosilicate (TEOS) is in ultrasound Ripple shakes 100 DEG C of 2h removal of impurities of oil bath;
Step 4, by 3g MTMSs (MTMOS), 0.5g palladium nitrates are added to by 6g isopropanols and 5ml just Solution B, 100 DEG C of oil bath 2h of magnetic agitation are formed in the mixed solution of silester (TEOS) composition;
Step 5, solution A mixed with solution B, 100 DEG C of oil bath 4h of magnetic agitation;
Step 6, by above-mentioned mixed solution with microwave treatment 2h be modified;
Step 7, using flame spraying one-step synthesis Pd-Me-HMS molecular sieves, i.e., above-mentioned solution is added to flame spray In the needle tubing of injection device, then add the CH4 of high heating value, and be passed through oxygen, while igniting by obtained solution from pin hole with The form of ion ejects the rapid synthesis Pd-Me-HMS molecular sieves at 3000 DEG C;
Step 8 and then the centrifugation under centrifugal separator, are dried, and are finally forged in Muffle furnace under sufficient air atmosphere 6h is burnt, Pd-Me-HMS molecular sieves are obtained;
Step 9, by obtained Pd-Me-HMS molecular sieves under sampling machine sample preparation into 30-60 mesh;
Step 10, obtained Pd-Me-HMS molecular sieves are urged by inlaying attachment method and be embedded on cup inwall, with stainless The granular Pd-Me-HMS molecular sieves of wire perforation, are then woven in the centre of lautertuns above cup.
Embodiment 7 produces palladium nitrate, MTMS (MTMOS) mass ratio 1:7 sample.0.5g palladium nitrates, 3.5g MTMSs (MTMOS), 10ml ethanol, 5ml tetraethyl orthosilicates, 8g hexadecylamines (HDA), 6g isopropanols, 200ml deionized waters.
Step 1, by 8g hexadecylamines (HDA) and 10ml ethanol, 100 DEG C of oil bath ultrasound 3h are removed under ultrasonic oscillation first It is miscellaneous;
Formed in step 2, the solution for being made up of 8g hexadecylamines (HDA) addition 200ml deionized waters and 10ml ethanol Solution A, 100 DEG C of oil bath ultrasound 3h of magnetic agitation;
Step 3, by MTMS (MTMOS), palladium nitrate, isopropanol, tetraethyl orthosilicate (TEOS) is in ultrasound Ripple shakes 100 DEG C of 2h removal of impurities of oil bath;
Step 4, by 3.5g MTMSs (MTMOS), 0.5g palladium nitrates are added to by 6g isopropanols and 5ml Solution B, 100 DEG C of oil bath 2h of magnetic agitation are formed in the mixed solution of tetraethyl orthosilicate (TEOS) composition;
Step 5, solution A mixed with solution B, 100 DEG C of oil bath 4h of magnetic agitation;
Step 6, by above-mentioned mixed solution with microwave treatment 2h be modified;
Step 7, using flame spraying one-step synthesis Pd-Me-HMS molecular sieves, i.e., above-mentioned solution is added to flame spray In the needle tubing of injection device, then add the CH4 of high heating value, and be passed through oxygen, while igniting by obtained solution from pin hole with The form of ion ejects the rapid synthesis Pd-Me-HMS molecular sieves at 3000 DEG C;
Step 8 and then the centrifugation under centrifugal separator, are dried, and are finally forged in Muffle furnace under sufficient air atmosphere 6h is burnt, Pd-Me-HMS molecular sieves are obtained;
Step 9, by obtained Pd-Me-HMS molecular sieves under sampling machine sample preparation into 30-60 mesh;
Step 10, obtained Pd-Me-HMS molecular sieves are urged by inlaying attachment method and be embedded on cup inwall, with stainless The granular Pd-Me-HMS molecular sieves of wire perforation, are then woven in the centre of lautertuns above cup.
Embodiment 8 produces palladium nitrate, MTMS (MTMOS) mass ratio 1:8 sample.0.5g palladium nitrates, 4g MTMS (MTMOS), 10ml ethanol, 5ml tetraethyl orthosilicates, 8g hexadecylamines (HDA), 6g isopropanols, 200ml Deionized water.
Step 1, by 8g hexadecylamines (HDA) and 10ml ethanol, 100 DEG C of oil bath ultrasound 3h are removed under ultrasonic oscillation first It is miscellaneous;
Formed in step 2, the solution for being made up of 8g hexadecylamines (HDA) addition 200ml deionized waters and 10ml ethanol Solution A, 100 DEG C of oil bath ultrasound 3h of magnetic agitation;
Step 3, by MTMS (MTMOS), palladium nitrate, isopropanol, tetraethyl orthosilicate (TEOS) is in ultrasound Ripple shakes 100 DEG C of 2h removal of impurities of oil bath;
Step 4, by 4g MTMSs (MTMOS), 0.5g palladium nitrates are added to by 6g isopropanols and 5ml just Solution B, 100 DEG C of oil bath 2h of magnetic agitation are formed in the mixed solution of silester (TEOS) composition;
Step 5, solution A mixed with solution B, 100 DEG C of oil bath 4h of magnetic agitation;
Step 6, by above-mentioned mixed solution with microwave treatment 2h be modified;
Step 7, using flame spraying one-step synthesis Pd-Me-HMS molecular sieves, i.e., above-mentioned solution is added to flame spray In the needle tubing of injection device, then add the CH4 of high heating value, and be passed through oxygen, while igniting by obtained solution from pin hole with The form of ion ejects the rapid synthesis Pd-Me-HMS molecular sieves at 3000 DEG C;
Step 8 and then the centrifugation under centrifugal separator, are dried, and are finally forged in Muffle furnace under sufficient air atmosphere 6h is burnt, Pd-Me-HMS molecular sieves are obtained;
Step 9, by obtained Pd-Me-HMS molecular sieves under sampling machine sample preparation into 30-60 mesh;
Step 10, obtained Pd-Me-HMS molecular sieves are urged by inlaying attachment method and be embedded on cup inwall, with stainless The granular Pd-Me-HMS molecular sieves of wire perforation, are then woven in the centre of lautertuns above cup.
Embodiment 9 produces palladium nitrate, MTMS (MTMOS) mass ratio 1:9 sample.0.5g palladium nitrates, 4.5g MTMSs (MTMOS), 10ml ethanol, 5ml tetraethyl orthosilicates, 8g hexadecylamines (HDA), 6g isopropanols, 200ml deionized waters.
Step 1, by 8g hexadecylamines (HDA) and 10ml ethanol, 100 DEG C of oil bath ultrasound 3h are removed under ultrasonic oscillation first It is miscellaneous;
Formed in step 2, the solution for being made up of 8g hexadecylamines (HDA) addition 200ml deionized waters and 10ml ethanol Solution A, 100 DEG C of oil bath ultrasound 3h of magnetic agitation;
Step 3, by MTMS (MTMOS), palladium nitrate, isopropanol, tetraethyl orthosilicate (TEOS) is in ultrasound Ripple shakes 100 DEG C of 2h removal of impurities of oil bath;
Step 4, by 4.5g MTMSs (MTMOS), 0.5g palladium nitrates are added to by 6g isopropanols and 5ml Solution B, 100 DEG C of oil bath 2h of magnetic agitation are formed in the mixed solution of tetraethyl orthosilicate (TEOS) composition;
Step 5, solution A mixed with solution B, 100 DEG C of oil bath 4h of magnetic agitation;
Step 6, by above-mentioned mixed solution with microwave treatment 2h be modified;
Step 7, using flame spraying one-step synthesis Pd-Me-HMS molecular sieves, i.e., above-mentioned solution is added to flame spray In the needle tubing of injection device, then add the CH4 of high heating value, and be passed through oxygen, while igniting by obtained solution from pin hole with The form of ion ejects the rapid synthesis Pd-Me-HMS molecular sieves at 3000 DEG C;
Step 8 and then the centrifugation under centrifugal separator, are dried, and are finally forged in Muffle furnace under sufficient air atmosphere 6h is burnt, Pd-Me-HMS molecular sieves are obtained;
Step 9, by obtained Pd-Me-HMS molecular sieves under sampling machine sample preparation into 30-60 mesh;
Step 10, obtained Pd-Me-HMS molecular sieves are urged by inlaying attachment method and be embedded on cup inwall, with stainless The granular Pd-Me-HMS molecular sieves of wire perforation, are then woven in the centre of lautertuns above cup.
Embodiment 10 produces palladium nitrate, MTMS (MTMOS) mass ratio 1:10 sample.0.5g palladium nitrates, 5g MTMSs (MTMOS), 10ml ethanol, 5ml tetraethyl orthosilicates, 8g hexadecylamines (HDA), 6g isopropanols, 200ml deionized waters.
Step 1, by 8g hexadecylamines (HDA) and 10ml ethanol, 100 DEG C of oil bath ultrasound 3h are removed under ultrasonic oscillation first It is miscellaneous;
Formed in step 2, the solution for being made up of 8g hexadecylamines (HDA) addition 200ml deionized waters and 10ml ethanol Solution A, 100 DEG C of oil bath ultrasound 3h of magnetic agitation;
Step 3, by MTMS (MTMOS), palladium nitrate, isopropanol, tetraethyl orthosilicate (TEOS) is in ultrasound Ripple shakes 100 DEG C of 2h removal of impurities of oil bath;
Step 4, by 5g MTMSs (MTMOS), 0.5g palladium nitrates are added to by 6g isopropanols and 5ml just Solution B, 100 DEG C of oil bath 2h of magnetic agitation are formed in the mixed solution of silester (TEOS) composition;
Step 5, solution A mixed with solution B, 100 DEG C of oil bath 4h of magnetic agitation;
Step 6, by above-mentioned mixed solution with microwave treatment 2h be modified;
Step 7, using flame spraying one-step synthesis Pd-Me-HMS molecular sieves, i.e., above-mentioned solution is added to flame spray In the needle tubing of injection device, then add the CH4 of high heating value, and be passed through oxygen, while igniting by obtained solution from pin hole with The form of ion ejects the rapid synthesis Pd-Me-HMS molecular sieves at 3000 DEG C;
Step 8 and then the centrifugation under centrifugal separator, are dried, and are finally forged in Muffle furnace under sufficient air atmosphere 6h is burnt, Pd-Me-HMS molecular sieves are obtained;
Step 9, by obtained Pd-Me-HMS molecular sieves under sampling machine sample preparation into 30-60 mesh;
Step 10, obtained Pd-Me-HMS molecular sieves are urged by inlaying attachment method and be embedded on cup inwall, with stainless The granular Pd-Me-HMS molecular sieves of wire perforation, are then woven in the centre of lautertuns above cup.
Embodiment 11 produces palladium nitrate, MTMS (MTMOS) mass ratio 1:11 sample.0.5g palladium nitrates, 5.5g MTMSs (MTMOS), 10ml ethanol, 5ml tetraethyl orthosilicates, 8g hexadecylamines (HDA), 6g isopropanols, 200ml deionized waters.
Step 1, by 8g hexadecylamines (HDA) and 10ml ethanol, 100 DEG C of oil bath ultrasound 3h are removed under ultrasonic oscillation first It is miscellaneous;
Formed in step 2, the solution for being made up of 8g hexadecylamines (HDA) addition 200ml deionized waters and 10ml ethanol Solution A, 100 DEG C of oil bath ultrasound 3h of magnetic agitation;
Step 3, by MTMS (MTMOS), palladium nitrate, isopropanol, tetraethyl orthosilicate (TEOS) is in ultrasound Ripple shakes 100 DEG C of 2h removal of impurities of oil bath;
Step 4, by 5.5g MTMSs (MTMOS), 0.5g palladium nitrates are added to by 6g isopropanols and 5ml Solution B, 100 DEG C of oil bath 2h of magnetic agitation are formed in the mixed solution of tetraethyl orthosilicate (TEOS) composition;
Step 5, solution A mixed with solution B, 100 DEG C of oil bath 4h of magnetic agitation;
Step 6, by above-mentioned mixed solution with microwave treatment 2h be modified;
Step 7, using flame spraying one-step synthesis Pd-Me-HMS molecular sieves, i.e., above-mentioned solution is added to flame spray In the needle tubing of injection device, then add the CH4 of high heating value, and be passed through oxygen, while igniting by obtained solution from pin hole with The form of ion ejects the rapid synthesis Pd-Me-HMS molecular sieves at 3000 DEG C;
Step 8 and then the centrifugation under centrifugal separator, are dried, and are finally forged in Muffle furnace under sufficient air atmosphere 6h is burnt, Pd-Me-HMS molecular sieves are obtained;
Step 9, by obtained Pd-Me-HMS molecular sieves under sampling machine sample preparation into 30-60 mesh;
Step 10, obtained Pd-Me-HMS molecular sieves are urged by inlaying attachment method and be embedded on cup inwall, with stainless The granular Pd-Me-HMS molecular sieves of wire perforation, are then woven in the centre of lautertuns above cup.
Embodiment 12 produces palladium nitrate, MTMS (MTMOS) mass ratio 1:12 sample.0.5g palladium nitrates, 6g MTMSs (MTMOS), 10ml ethanol, 5ml tetraethyl orthosilicates, 8g hexadecylamines (HDA), 6g isopropanols, 200ml deionized waters.
Step 1, by 8g hexadecylamines (HDA) and 10ml ethanol, 100 DEG C of oil bath ultrasound 3h are removed under ultrasonic oscillation first It is miscellaneous;
Formed in step 2, the solution for being made up of 8g hexadecylamines (HDA) addition 200ml deionized waters and 10ml ethanol Solution A, 100 DEG C of oil bath ultrasound 3h of magnetic agitation;
Step 3, by MTMS (MTMOS), palladium nitrate, isopropanol, tetraethyl orthosilicate (TEOS) is in ultrasound Ripple shakes 100 DEG C of 2h removal of impurities of oil bath;
Step 4, by 6g MTMSs (MTMOS), 0.5g palladium nitrates are added to by 6g isopropanols and 5ml just Solution B, 100 DEG C of oil bath 2h of magnetic agitation are formed in the mixed solution of silester (TEOS) composition;
Step 5, solution A mixed with solution B, 100 DEG C of oil bath 4h of magnetic agitation;
Step 6, by above-mentioned mixed solution with microwave treatment 2h be modified;
Step 7, using flame spraying one-step synthesis Pd-Me-HMS molecular sieves, i.e., above-mentioned solution is added to flame spray In the needle tubing of injection device, then add the CH4 of high heating value, and be passed through oxygen, while igniting by obtained solution from pin hole with The form of ion ejects the rapid synthesis Pd-Me-HMS molecular sieves at 3000 DEG C;
Step 8 and then the centrifugation under centrifugal separator, are dried, and are finally forged in Muffle furnace under sufficient air atmosphere 6h is burnt, Pd-Me-HMS molecular sieves are obtained;
Step 9, by obtained Pd-Me-HMS molecular sieves under sampling machine sample preparation into 30-60 mesh;
Step 10, obtained Pd-Me-HMS molecular sieves are urged by inlaying attachment method and be embedded on cup inwall, with stainless The granular Pd-Me-HMS molecular sieves of wire perforation, are then woven in the centre of lautertuns above cup.
Embodiment 13 produces palladium nitrate, MTMS (MTMOS) mass ratio 1:13 sample.0.5g palladium nitrates, 6.5g MTMSs (MTMOS), 10ml ethanol, 5ml tetraethyl orthosilicates, 8g hexadecylamines (HDA), 6g isopropanols, 200ml deionized waters.
Step 1, by 8g hexadecylamines (HDA) and 10ml ethanol, 100 DEG C of oil bath ultrasound 3h are removed under ultrasonic oscillation first It is miscellaneous;
Formed in step 2, the solution for being made up of 8g hexadecylamines (HDA) addition 200ml deionized waters and 10ml ethanol Solution A, 100 DEG C of oil bath ultrasound 3h of magnetic agitation;
Step 3, by MTMS (MTMOS), palladium nitrate, isopropanol, tetraethyl orthosilicate (TEOS) is in ultrasound Ripple shakes 100 DEG C of 2h removal of impurities of oil bath;
Step 4, by 6.5g MTMSs (MTMOS), 0.5g palladium nitrates are added to by 6g isopropanols and 5ml Solution B, 100 DEG C of oil bath 2h of magnetic agitation are formed in the mixed solution of tetraethyl orthosilicate (TEOS) composition;
Step 5, solution A mixed with solution B, 100 DEG C of oil bath 4h of magnetic agitation;
Step 6, by above-mentioned mixed solution with microwave treatment 2h be modified;
Step 7, using flame spraying one-step synthesis Pd-Me-HMS molecular sieves, i.e., above-mentioned solution is added to flame spray In the needle tubing of injection device, then add the CH4 of high heating value, and be passed through oxygen, while igniting by obtained solution from pin hole with The form of ion ejects the rapid synthesis Pd-Me-HMS molecular sieves at 3000 DEG C;
Step 8 and then the centrifugation under centrifugal separator, are dried, and are finally forged in Muffle furnace under sufficient air atmosphere 6h is burnt, Pd-Me-HMS molecular sieves are obtained;
Step 9, by obtained Pd-Me-HMS molecular sieves under sampling machine sample preparation into 30-60 mesh;
Step 10, obtained Pd-Me-HMS molecular sieves are urged by inlaying attachment method and be embedded on cup inwall, with stainless The granular Pd-Me-HMS molecular sieves of wire perforation, are then woven in the centre of lautertuns above cup.
Embodiment 14 produces palladium nitrate, MTMS (MTMOS) mass ratio 1:14 sample.0.5g palladium nitrates, 7g MTMSs (MTMOS), 10ml ethanol, 5ml tetraethyl orthosilicates, 8g hexadecylamines (HDA), 6g isopropanols, 200ml deionized waters.
Step 1, by 8g hexadecylamines (HDA) and 10ml ethanol, 100 DEG C of oil bath ultrasound 3h are removed under ultrasonic oscillation first It is miscellaneous;
Formed in step 2, the solution for being made up of 8g hexadecylamines (HDA) addition 200ml deionized waters and 10ml ethanol Solution A, 100 DEG C of oil bath ultrasound 3h of magnetic agitation;
Step 3, by MTMS (MTMOS), palladium nitrate, isopropanol, tetraethyl orthosilicate (TEOS) is in ultrasound Ripple shakes 100 DEG C of 2h removal of impurities of oil bath;
Step 4, by 7g MTMSs (MTMOS), 0.5g palladium nitrates are added to by 6g isopropanols and 5ml just Solution B, 100 DEG C of oil bath 2h of magnetic agitation are formed in the mixed solution of silester (TEOS) composition;
Step 5, solution A mixed with solution B, 100 DEG C of oil bath 4h of magnetic agitation;
Step 6, by above-mentioned mixed solution with microwave treatment 2h be modified;
Step 7, using flame spraying one-step synthesis Pd-Me-HMS molecular sieves, i.e., above-mentioned solution is added to flame spray In the needle tubing of injection device, then add the CH4 of high heating value, and be passed through oxygen, while igniting by obtained solution from pin hole with The form of ion ejects the rapid synthesis Pd-Me-HMS molecular sieves at 3000 DEG C;
Step 8 and then the centrifugation under centrifugal separator, are dried, and are finally forged in Muffle furnace under sufficient air atmosphere 6h is burnt, Pd-Me-HMS molecular sieves are obtained;
Step 9, by obtained Pd-Me-HMS molecular sieves under sampling machine sample preparation into 30-60 mesh;
Step 10, obtained Pd-Me-HMS molecular sieves are urged by inlaying attachment method and be embedded on cup inwall, with stainless The granular Pd-Me-HMS molecular sieves of wire perforation, are then woven in the centre of lautertuns above cup.
Reference examples 1 produce palladium nitrate, MTMS (MTMOS) mass ratio 1:10 sample.0.5g palladium nitrates, 5g MTMS (MTMOS), 10ml ethanol, 5ml tetraethyl orthosilicates, 8g hexadecylamines (HDA), 6g isopropanols, 200ml Deionized water.
Step 1,100 DEG C of oil bath ultrasound 3h removal of impurities under common concussion by 8g hexadecylamines (HDA) and 10ml ethanol first;
Formed in step 2, the solution for being made up of 8g hexadecylamines (HDA) addition 200ml deionized waters and 10ml ethanol Solution A, 100 DEG C of oil bath ultrasound 3h of magnetic agitation;
Step 3, by MTMS (MTMOS), palladium nitrate, isopropanol, tetraethyl orthosilicate (TEOS) is common Shake 100 DEG C of 2h removal of impurities of oil bath;
Step 4, by 5g MTMSs (MTMOS), 0.5g palladium nitrates are added to by 6g isopropanols and 5ml just Solution B, 100 DEG C of oil bath 2h of magnetic agitation are formed in the mixed solution of silester (TEOS) composition;
Step 5, solution A mixed with solution B, 100 DEG C of oil bath 4h of magnetic agitation;
Step 6, by above-mentioned mixed solution with microwave treatment 2h be modified;
Step 7, using flame spraying one-step synthesis Pd-Me-HMS molecular sieves, i.e., above-mentioned solution is added to flame spray In the needle tubing of injection device, then add the CH4 of high heating value, and be passed through oxygen, while igniting by obtained solution from pin hole with The form of ion ejects the rapid synthesis Pd-Me-HMS molecular sieves at 3000 DEG C;
Step 8 and then the centrifugation under centrifugal separator, are dried, and are finally forged in Muffle furnace under sufficient air atmosphere 6h is burnt, Pd-Me-HMS molecular sieves are obtained;
Step 9, by obtained Pd-Me-HMS molecular sieves under sampling machine sample preparation into 30-60 mesh;
Step 10, obtained Pd-Me-HMS molecular sieves are urged by inlaying attachment method and be embedded on cup inwall, with stainless The granular Pd-Me-HMS molecular sieves of wire perforation, are then woven in the centre of lautertuns above cup.
Reference examples 2 produce palladium nitrate, MTMS (MTMOS) mass ratio 1:10 sample.0.5g palladium nitrates, 5g MTMS (MTMOS), 10ml ethanol, 5ml tetraethyl orthosilicates, 8g hexadecylamines (HDA), 6g isopropanols, 200ml Deionized water.
Step 1, by 8g hexadecylamines (HDA) and 10ml ethanol, 100 DEG C of oil bath ultrasound 3h are removed under ultrasonic oscillation first It is miscellaneous;
Formed in step 2, the solution for being made up of 8g hexadecylamines (HDA) addition 200ml deionized waters and 10ml ethanol Solution A, stirs 100 DEG C of oil bath ultrasound 3h;
Step 3, by MTMS (MTMOS), palladium nitrate, isopropanol, tetraethyl orthosilicate (TEOS) is in ultrasound Ripple shakes 100 DEG C of 2h removal of impurities of oil bath;
Step 4, by 5g MTMSs (MTMOS), 0.5g palladium nitrates are added to by 6g isopropanols and 5ml just Solution B is formed in the mixed solution of silester (TEOS) composition, 100 DEG C of oil bath 2h are stirred;
Step 5, solution A mixed with solution B, 100 DEG C of oil bath 4h of magnetic agitation;
Step 6, by above-mentioned mixed solution with microwave treatment 2h be modified;
Step 7, using flame spraying one-step synthesis Pd-Me-HMS molecular sieves, i.e., above-mentioned solution is added to flame spray In the needle tubing of injection device, then add the CH4 of high heating value, and be passed through oxygen, while igniting by obtained solution from pin hole with The form of ion ejects the rapid synthesis Pd-Me-HMS molecular sieves at 3000 DEG C;
Step 8 and then the centrifugation under centrifugal separator, are dried, and are finally forged in Muffle furnace under sufficient air atmosphere 6h is burnt, Pd-Me-HMS molecular sieves are obtained;
Step 9, by obtained Pd-Me-HMS molecular sieves under sampling machine sample preparation into 30-60 mesh;
Step 10, obtained Pd-Me-HMS molecular sieves are urged by inlaying attachment method and be embedded on cup inwall, with stainless The granular Pd-Me-HMS molecular sieves of wire perforation, are then woven in the centre of lautertuns above cup.
Reference examples 3 produce palladium nitrate, MTMS (MTMOS) mass ratio 1:10 sample.0.5g palladium nitrates, 5g MTMS (MTMOS), 10ml ethanol, 5ml tetraethyl orthosilicates, 8g hexadecylamines (HDA), 6g isopropanols, 200ml Deionized water.
Step 1, by 8g hexadecylamines (HDA) and 10ml ethanol, 100 DEG C of oil bath ultrasound 3h are removed under ultrasonic oscillation first It is miscellaneous;
Formed in step 2, the solution for being made up of 8g hexadecylamines (HDA) addition 200ml deionized waters and 10ml ethanol Solution A, 100 DEG C of oil bath ultrasound 3h of magnetic agitation;
Step 3, by MTMS (MTMOS), palladium nitrate, isopropanol, tetraethyl orthosilicate (TEOS) is in ultrasound Ripple shakes 100 DEG C of 2h removal of impurities of oil bath;
Step 4, by 5g MTMSs (MTMOS), 0.5g palladium nitrates are added to by 6g isopropanols and 5ml just Solution B, 100 DEG C of oil bath 2h of magnetic agitation are formed in the mixed solution of silester (TEOS) composition;
Step 5, solution A mixed with solution B, 100 DEG C of oil bath 4h of magnetic agitation;
Step 6, using flame spraying one-step synthesis Pd-Me-HMS molecular sieves, i.e., above-mentioned solution is added to flame spray In the needle tubing of injection device, then add the CH4 of high heating value, and be passed through oxygen, while igniting by obtained solution from pin hole with The form of ion ejects the rapid synthesis Pd-Me-HMS molecular sieves at 3000 DEG C;
Step 7 and then the centrifugation under centrifugal separator, are dried, and are finally forged in Muffle furnace under sufficient air atmosphere 6h is burnt, Pd-Me-HMS molecular sieves are obtained;
Step 8, by obtained Pd-Me-HMS molecular sieves under sampling machine sample preparation into 30-60 mesh;
Step 9, obtained Pd-Me-HMS molecular sieves are urged by inlaying attachment method and be embedded on cup inwall, with stainless The granular Pd-Me-HMS molecular sieves of wire perforation, are then woven in the centre of lautertuns above cup.
Reference examples 4 produce the sample for being added without palladium nitrate modification.5g MTMSs (MTMOS), 10ml ethanol, 5ml tetraethyl orthosilicates, 8g hexadecylamines (HDA), 6g isopropanols, 200ml deionized waters.
Step 1, by 8g hexadecylamines (HDA) and 10ml ethanol, 100 DEG C of oil bath ultrasound 3h are removed under ultrasonic oscillation first It is miscellaneous;
Formed in step 2, the solution for being made up of 8g hexadecylamines (HDA) addition 200ml deionized waters and 10ml ethanol Solution A, 100 DEG C of oil bath ultrasound 3h of magnetic agitation;
Step 3, by MTMS (MTMOS), isopropanol, tetraethyl orthosilicate (TEOS) is in ultrasonic oscillation oil Bathe 100 DEG C of 2h removal of impurities;Step 4, by 5g MTMSs (MTMOS), be added to by 6g isopropanols and the positive silicic acid second of 5ml Solution B, 100 DEG C of oil bath 2h of magnetic agitation are formed in the mixed solution of ester (TEOS) composition;
Step 5, solution A mixed with solution B, 100 DEG C of oil bath 4h of magnetic agitation;
Step 6, by above-mentioned mixed solution with microwave treatment 2h be modified;
Step 7, using flame spraying one-step synthesis Me-HMS molecular sieves, i.e., above-mentioned solution is added to flame injection dress In the needle tubing put, then add the CH4 of high heating value, and be passed through oxygen, while igniting by obtained solution from pin hole with ion Form eject at 3000 DEG C rapid synthesis Me-HMS molecular sieves;
Step 8 and then the centrifugation under centrifugal separator, are dried, and are finally forged in Muffle furnace under sufficient air atmosphere 6h is burnt, Me-HMS molecular sieves are obtained;
Step 9, by obtained Me-HMS molecular sieves under sampling machine sample preparation into 30-60 mesh;
Step 10, obtained Pd-Me-HMS molecular sieves are urged by inlaying attachment method and be embedded on cup inwall, with stainless The granular Me-HMS molecular sieves of wire perforation, are then woven in the centre of lautertuns above cup.
Adsorption cleaning running water effect assessment
The Pd-Me-HMS molecular sieve cups of obtained various ratios are unified into volume 500ml, by same tap with for the moment Carve the water that takes and fill each cup, do the common cup inwall of one group of blank assay group and notch does not add the molecule of my invention Sieve.5min is stood, the indices of water are then detected.
The Testing index of this research of Testing index and the method for inspection, with reference to the Ministry of Public Health for water purifier security and function Property evaluate correlation
Standard, specifically includes purified water heavy metal index (iron, manganese, copper, zinc, lead, arsenic), general chemical index [oxygen demand Clearance, acid-base value (pH value), colourity, turbidity] and microbiological indicator (total plate count, total coli group).It is net because that need to calculate Hydrophone therefore adds the oxygen demand for surveying municipal water, oxygen demand clearance=(municipal water consume oxygen amount-purification for the clearance of oxygen demand Water consume oxygen amount)/municipal administration water consume oxygen amount × 100%.
Test result indicates that Pd-Me-HMS molecular sieves prepared by embodiment 9,10 are used in cup in adsorption cleaning running water Metal impurities and other effects preferably, illustrate in palladium nitrate, MTMS (MTMOS) mass ratio 1:9,1:When 10 Synergy between them is best, and at most, the narrower absorption in duct is most with stronger for the acidic site in molecular sieve.Under other ratios Pd-Me-HMS molecular sieves are made, and for there is certain adsorption capacity in cup, still effect is bad.Row 10, comparative example are implemented in contrast 1,2,3,4 can be found that.Without magnetic agitation, ultrasonic oscillation, microwave treatment is added without the element modified obtained Pd- of Pd It is bad that Me-HMS, Me-HMS molecular sieve are used for cup adsorption cleaning running water effect.

Claims (2)

1. a kind of be used for the Pd-Me-HMS molecular sieve preparation methods of the metal impurities in cup in adsorption cleaning running water, it is special Levy and be, respectively with hexadecylamine (HDA), MTMS (MTMOS), palladium nitrate, isopropanol, tetraethyl orthosilicate (TEOS) ethanol, the raw material such as ammonium chloride water is by magnetization, the Pd-Me-HMS molecules that the modified method such as ultrasonic oscillation is prepared Sieve.
2. a kind of Pd-Me-HMS of metal impurities in adsorption cleaning running water in cup according to claim 1 Molecular sieve preparation method, it is characterised in that specific method is as follows:
Step 1,100 DEG C of oil bath ultrasound 3h removal of impurities under ultrasonic oscillation by hexadecylamine (HDA) and ethanol first;
Solution A, magnetic agitation are formed in step 2, the solution for being made up of hexadecylamine (HDA) addition deionized water and ethanol 100 DEG C of oil bath ultrasound 3h;
Step 3, by MTMS (MTMOS), palladium nitrate, isopropanol, tetraethyl orthosilicate (TEOS) shakes in ultrasonic wave Swing 100 DEG C of 2h removal of impurities of oil bath;
Step 4, by MTMS (MTMOS), palladium nitrate is added to by isopropanol and tetraethyl orthosilicate (TEOS) group Into mixed solution in form solution B, 100 DEG C of oil bath 2h of magnetic agitation;
Step 5, solution A mixed with solution B, 100 DEG C of oil bath 4h of magnetic agitation;
Step 6, by above-mentioned mixed solution with microwave treatment 2h be modified:
Step 7, using flame spraying one-step synthesis Pd-Me-HMS molecular sieves, i.e., above-mentioned solution is added to flame injection dress In the needle tubing put, then add the CH4 of high heating value, and be passed through oxygen, while igniting by obtained solution from pin hole with ion Form eject at 3000 DEG C rapid synthesis Pd-Me-HMS molecular sieves;
Step 8 and then the centrifugation under centrifugal separator, are dried, and finally calcine 6h under sufficient air atmosphere in Muffle furnace, Obtain Pd-Me-HMS molecular sieves;
Step 9, by obtained Pd-Me-HMS molecular sieves under sampling machine sample preparation into 30-60 mesh;
Step 10, obtained Pd-Me-HMS molecular sieves are urged by inlaying attachment method and be embedded on cup inwall, use stainless steel wire The granular Pd-Me-HMS molecular sieves of line perforation, are then woven in the centre of lautertuns above cup.
CN201710301014.0A 2017-05-02 2017-05-02 It is a kind of to be used for the Pd Me HMS molecular sieve preparation methods of the metal impurities in cup in adsorption cleaning running water Pending CN107096503A (en)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106308346A (en) * 2016-10-30 2017-01-11 宁波科邦华诚技术转移服务有限公司 Embedded filter box cup
CN106673113A (en) * 2017-03-01 2017-05-17 宁波圆明工业设计有限公司 Purifying kettle

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106308346A (en) * 2016-10-30 2017-01-11 宁波科邦华诚技术转移服务有限公司 Embedded filter box cup
CN106673113A (en) * 2017-03-01 2017-05-17 宁波圆明工业设计有限公司 Purifying kettle

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