CN105565334A - High-separation oxygen generation molecular sieve and preparation method thereof - Google Patents

Abstract

The invention discloses a high-separation oxygen generation molecular sieve and a preparation method thereof. The high-separation oxygen generation molecular sieve is prepared from, by weight, 21-27 parts of bryozoatum, 16-22 parts of bauxite, 15-20 parts of kaliophilite, 11-18 parts of illite, 13-19 parts of coal ash, 19-26 parts of rectorite, 22-28 parts of imvite, 5-10 parts of calcium silicate, 55-65 parts of sodium hydroxide, 30-40 parts of sodium metaaluminate, 20-25 parts of sodium metasilicate nonahydrate and 14-18 parts of a seeding director. The obtained molecular sieve is good in nitrogen and oxygen separation performance which is five times or higher than that of a traditional molecular sieve, has the good mechanical strength and adsorption capacity, can be widely applied to a pressure swing adsorption oxygen generation device and is wide in market prospect.

Description

A kind of high score is from oxygen molecular sieve and preparation method thereof

Technical field

The present invention relates to a kind of molecular sieve and preparation method thereof, be specifically related to a kind of high score from oxygen molecular sieve and preparation method thereof.

Background technology

In recent years, due to the exploitation of oxygen adsorbent of molecular sieve and updating of technical process, omnibus control system technology is rapidly developed.Separating oxygen from air by means of pressure swing adsorption process has short, the feature such as the construction period is short, running cost is low, level of automation is high, maintenance is simple, comprehensive energy consumption is low start time, is widely used in the fields such as iron and steel, nonferrous metallurgy, chemical industry, furnace energy-saving, environmental protection, glass, papermaking, medical treatment.

Total institute is known, and adsorbent of molecular sieve is the key core of omnibus control system technology, and the performance of adsorbent of molecular sieve directly decides the investment of device, and volume weight and unit produce the integrated performance index such as oxygen rate and gas consumption.Molecular sieve in the market for pressure swing adsorption oxygen making device is of a great variety, but mostly there is the shortcoming of nitrogen oxygen separating poor performance, thus affects the final separating effect of pressure swing adsorption oxygen making device.

Summary of the invention

The object of the invention is to for the deficiencies in the prior art, provide a kind of high score from oxygen molecular sieve and preparation method thereof.

For realizing your object above-mentioned, the present invention adopts following technical scheme:

A kind of high score, from oxygen molecular sieve, is made up of the raw material of following weight part: Pumice 21-27, bauxitic clay 16-22, kaliophylite 15-20, illite 11-18, flyash 13-19, rectorite leng 19-26, polynite 22-28, Calucium Silicate powder 5-10, sodium hydroxide 55-65, sodium metaaluminate 30-40, nine water water glass 20-25, seeding director 14-18;

The preparation method of described seeding director is as follows: a, get the raw material of following weight part: Pumice 15-20, rectorite leng 12-16, polynite 10-15, non-hydrate sodium metasilicate 20-25, sodium hydroxide 14-18, sodium metaaluminate 7-11; B, Pumice, rectorite leng, polynite to be mixed, 600-650 DEG C of calcining 1-2h, the sulphuric acid soln be ratio and the volumetric molar concentration of 1:16-22 according to solid-to-liquid ratio after naturally cooling to normal temperature being 2mol/L mixes, heating in water bath is to 70-80 DEG C, insulation 35-45min, filters, washing, dry, 740-780 DEG C of calcining 1.5-2.5h, naturally cools to normal temperature, pulverizes, grinding, crosses 200-300 mesh sieve; C, get sodium hydroxide and be dissolved in the deionized water being equivalent to its 12-16 times amount, then the powder that step b is obtained is added, under the condition stirred, non-hydrate sodium metasilicate and sodium metaaluminate is added after mixing, at 65-75 DEG C, 1-2h is heated after mixing, water-cooled is to normal temperature, more still aging 18-24h and get final product.

High score, from a preparation method for oxygen molecular sieve, comprises the following steps:

(1) Pumice, bauxitic clay, flyash, Calucium Silicate powder are mixed, pulverize, cross 150-250 mesh sieve, then be that the powder after sieving is joined volumetric molar concentration is in the sulphuric acid soln of 1mol/L for the ratio of 1:10-15 according to solid-to-liquid ratio, heating in water bath to 75-85 DEG C, ultrasonic disperse 20-30min, filter, washing, dries, stand-by;

(2) kaliophylite, illite, rectorite leng, polynite are mixed, 810-850 DEG C of calcining 2-3h, naturally cools to normal temperature, pulverizes, cross 200-300 mesh sieve, stand-by;

(3) powder obtained with step (2) for powder obtained for step (1) is mixed, add appropriate deionized water and make the suspension that concentration is 45-50%, microwave treatment 25-35min, microwave power is 200-400W, magnetic agitation 20-30min again, rotating speed is 2000-3000r/min, is then spray dried to powder, stand-by;

(4) sodium hydroxide, sodium metaaluminate, nine water water glass are mixed, then the deionized water being equivalent to mixture 10-15 times amount is added, the powder that step (3) is obtained is added again after stirring, 3-5h is stirred at 70-80 DEG C, then still aging 12-24h, then add seeding director, heating in water bath is to 95-105 DEG C, stirring reaction 5-8h, be warming up to 110-130 DEG C again, thermostatic crystallization 12-18h, after reaction terminates, filter, being washed to filter residue pH value is 7-8, then dries, grinding, sieve, get product.

Beneficial effect of the present invention:

The molecular sieve nitrogen oxygen separating performance that the present invention obtains is good, is more than 5 times of conventional molecular sieve, has good physical strength and loading capacity simultaneously, can be widely used in pressure swing adsorption oxygen making device, wide market.

Embodiment

A kind of high score, from oxygen molecular sieve, is made up of the raw material of following weight (kg): Pumice 24, bauxitic clay 19, kaliophylite 17, illite 14, flyash 16, rectorite leng 23, polynite 26, Calucium Silicate powder 8, sodium hydroxide 60, sodium metaaluminate 35, nine water water glass 22, seeding director 16;

The preparation method of described seeding director is as follows: a, get the raw material of following weight (kg): Pumice 17, rectorite leng 13, polynite 12, non-hydrate sodium metasilicate 21, sodium hydroxide 15, sodium metaaluminate 9; B, Pumice, rectorite leng, polynite to be mixed, 630 DEG C of calcining 1.5h, the sulphuric acid soln be ratio and the volumetric molar concentration of 1:18 according to solid-to-liquid ratio after naturally cooling to normal temperature being 2mol/L mixes, heating in water bath to 75 DEG C, insulation 40min, filters, washing, dry, 760 DEG C of calcining 2h, naturally cool to normal temperature, pulverize, grinding, crosses 250 mesh sieves; C, get sodium hydroxide and be dissolved in the deionized water being equivalent to its 14 times amount, then add the powder that step b is obtained, under the condition stirred, add non-hydrate sodium metasilicate and sodium metaaluminate after mixing, after mixing, at 70 DEG C, heat 1-2h, water-cooled is to normal temperature, more still aging 20h and get final product.

High score, from a preparation method for oxygen molecular sieve, comprises the following steps:

(1) Pumice, bauxitic clay, flyash, Calucium Silicate powder are mixed, pulverize, cross 200 mesh sieves, then be that the powder after sieving is joined volumetric molar concentration is in the sulphuric acid soln of 1mol/L for the ratio of 1:12 according to solid-to-liquid ratio, heating in water bath to 80 DEG C, ultrasonic disperse 25min, filter, washing, dries, stand-by;

(2) kaliophylite, illite, rectorite leng, polynite are mixed, 820 DEG C of calcining 3h, naturally cool to normal temperature, pulverize, cross 250 mesh sieves, stand-by;

(3) powder obtained with step (2) for powder obtained for step (1) is mixed, add appropriate deionized water and make the suspension that concentration is 48%, microwave treatment 30min, microwave power is 300W, magnetic agitation 25min again, rotating speed is 2500r/min, is then spray dried to powder, stand-by;

(4) sodium hydroxide, sodium metaaluminate, nine water water glass are mixed, then add the deionized water being equivalent to mixture 13 times amount, after stirring, add the powder that step (3) is obtained again, at 75 DEG C, stir 3-5h, then still aging 15h, then add seeding director, heating in water bath to 100 DEG C, stirring reaction 6h, then be warming up to 120 DEG C, thermostatic crystallization 16h, after reaction terminates, filters, being washed to filter residue pH value is 7.5, then dries, grinding, sieve, get product.

The service check of the oxygen molecular sieve that above-described embodiment obtains the results are shown in Table 1.

The performance test results of table 1 oxygen molecular sieve

Project	Unit	Test result 2-->
			Tap density	g/ml	0.69
Ultimate compression strength	N	38
			Nitrogen equilibrium adsorptive capacity	ml/g	26
N 2/O 2Choosing coefficient	-	7.1

Claims (2)

1. a high score is from oxygen molecular sieve, it is characterized in that, be made up of the raw material of following weight part: Pumice 21-27, bauxitic clay 16-22, kaliophylite 15-20, illite 11-18, flyash 13-19, rectorite leng 19-26, polynite 22-28, Calucium Silicate powder 5-10, sodium hydroxide 55-65, sodium metaaluminate 30-40, nine water water glass 20-25, seeding director 14-18;

The preparation method of described seeding director is as follows: a, get the raw material of following weight part: Pumice 15-20, rectorite leng 12-16, polynite 10-15, non-hydrate sodium metasilicate 20-25, sodium hydroxide 14-18, sodium metaaluminate 7-11; B, Pumice, rectorite leng, polynite to be mixed, 600-650 DEG C of calcining 1-2h, the sulphuric acid soln be ratio and the volumetric molar concentration of 1:16-22 according to solid-to-liquid ratio after naturally cooling to normal temperature being 2mol/L mixes, heating in water bath is to 70-80 DEG C, insulation 35-45min, filters, washing, dry, 740-780 DEG C of calcining 1.5-2.5h, naturally cools to normal temperature, pulverizes, grinding, crosses 200-300 mesh sieve; C, get sodium hydroxide and be dissolved in the deionized water being equivalent to its 12-16 times amount, then the powder that step b is obtained is added, under the condition stirred, non-hydrate sodium metasilicate and sodium metaaluminate is added after mixing, at 65-75 DEG C, 1-2h is heated after mixing, water-cooled is to normal temperature, more still aging 18-24h and get final product.

2. high score as claimed in claim 1 is from a preparation method for oxygen molecular sieve, it is characterized in that, comprises the following steps:

(1) Pumice, bauxitic clay, flyash, Calucium Silicate powder are mixed, pulverize, cross 150-250 mesh sieve, then be that the powder after sieving is joined volumetric molar concentration is in the sulphuric acid soln of 1mol/L for the ratio of 1:10-15 according to solid-to-liquid ratio, heating in water bath to 75-85 DEG C, ultrasonic disperse 20-30min, filter, washing, dries, stand-by;

(2) kaliophylite, illite, rectorite leng, polynite are mixed, 810-850 DEG C of calcining 2-3h, naturally cools to normal temperature, pulverizes, cross 200-300 mesh sieve, stand-by;

(3) powder obtained with step (2) for powder obtained for step (1) is mixed, add appropriate deionized water and make the suspension that concentration is 45-50%, microwave treatment 25-35min, microwave power is 200-400W, magnetic agitation 20-30min again, rotating speed is 2000-3000r/min, is then spray dried to powder, stand-by;

(4) sodium hydroxide, sodium metaaluminate, nine water water glass are mixed, then the deionized water being equivalent to mixture 10-15 times amount is added, the powder that step (3) is obtained is added again after stirring, 3-5h is stirred at 70-80 DEG C, then still aging 12-24h, then add seeding director, heating in water bath is to 95-105 DEG C, stirring reaction 5-8h, be warming up to 110-130 DEG C again, thermostatic crystallization 12-18h, after reaction terminates, filter, being washed to filter residue pH value is 7-8, then dries, grinding, sieve, get product.