Static Wash, Cyclic Neutralization and Washing of 4A Zeolite

Alumina of our company is mainly produced by the sintering method. The high cost of the sintering method is known to all people. Under the market environment, we are faced with tremendous pressure to reduce costs. Our company has made the chemical alumina as the development focus and vigorously developed the chemical alumina. However, the development of chemical alumina has the problem of contradiction between chemical alumina and sintering method. How to realize the coordinated development of chemical alumina and sintering method is a problem that we face, namely, the optimization of chemicals and sintering methods. Not only the development of chemicals but also the cost reduction of the sintering process is the development direction of the development of chemicals. The most important contradiction is that due to the increase in the amount of chemicals used, the amount of alumina scrubbing water can not be balanced, affecting the production of alumina. Taking the current production workshop as an example, it adopts tape filter separation, static washing plus one-time scrubbing, washing water volume is about 6-7 tons, steam consumption is about 0.7 tons, and the cost is about 90-100 yuan/ton. Higher washing costs, it is necessary to reduce water consumption. Calculated at an annual output of 200,000 tons, about 1.4 million tons of water is fed into the water from the sintering process each year, which imposes a huge burden on the sintering process and seriously affects the balance of the sintering process water. In light of future development needs, the next step will continue to expand the production of 4A zeolite, and the contradiction in water consumption will be further intensified. Therefore, if the amount of water used for washing 4A zeolite can be effectively reduced, the production cost of 4A zeolite can be reduced, and the waste liquid discharge in the production process of 4A zeolite can be reduced; the water conflict with the sintering method can also be alleviated, and the water content obtained after washing can be reduced. Alkaline waste liquids can also be used more appropriately. It can be said that reducing the amount of washing water for 4A zeolites results in a win-win result and can save a lot of costs for the company.
L/S (dry basis) Static washing liquid composition (g/l) 4A Zeolite Product Indicator After Washing
NT AO Nc Calcium exchange Burn off pH
0.9 35.10 0.9 7.15 305 21.02 10.84
1.2 30.74 1.5 9.86 305 21.05 10.82
1.0 31.22 1.55 7.82 311 20.73 10.84
1.3 29.47 1.65 7.55 307 21.33 10.92
1.4 32.39 1.5 7.35 305 21.11 10.94
In the prior art, a large amount of hot water is used to leach a solid-liquid separated filter cake on a tape filter, and then the filter cake that has been washed away from most of the alkali is poured into a scrubbing tank to scrub, so the first step of the process is Determine the amount of static washing, that is, to find the amount of washing water and take the best alkali. Since all the components in the static washing solution come from the 4A zeolite solution, the attached solution is flushed into the static washing solution. Therefore, the composition of the static washing solution depends on the composition of the solution and the amount of static washing water. Therefore, other factors are maintained by controlling irrelevant factors. Similarly, monitoring the level of total alkali in the static washing solution obtained by static washing with different amounts of water can determine an optimum value, so that the elution of alkali is the most and the amount of washing water used is the least, and the most appropriate concentration of the static washing solution is obtained. A certain amount of 4A zeolite filter cake contains the amount of alkali Af, then washed with water after the alkali was divided into the residual alkali in the zeolite AC and was taken into the bath of the alkali AJ, namely: Af = AC + AJ
It can be seen from Table 1 that all indicators of 4A zeolite after scrubbing are qualified, but the calcium exchange is slightly high. This is because the product adds a small amount of sodium carbonate, but this does not affect the product quality, the product of sodium carbonate The increase in the content is due to the fact that the sodium carbonate in the scrubbing liquid is brought in by sodium bicarbonate. Through calculation and test verification, the total alkali and carbonic acid content in the scrubbing liquid in the test are determined, and the product is qualified under the precondition of ensuring the product. The added sodium carbonate quality is only 0.2%~0.4%, which is very insignificant. We compared the washed product with the current six workshop products and PQ samples. The results are shown in Table 2. From the results, we can see that there is no essence. difference.
In the existing 4A zeolite production plant, there is no need for major transformation. Simply install the flow meter in the static washing section, strictly control the amount of washing water and the amount of material to be washed. The second step of washing is changed to cyclic washing, and the CO2 pipeline is added to the water storage tank. The carbonation of the circulating washing liquid will reach the technical requirements of the circulating washing liquid.
On the tape filter, it is washed with industrial demineralized water, and the washing liquid is sent to the alumina plant. The tape filter cake was beaten with a circulating wash solution and sent to an OK filter press. The filtrate was recycled to the wash solution. The filtrate continuously passes CO2 to maintain a certain NaHCO3 concentration. The recirculating lotion does not need to be supplemented with fresh water and can be recycled. Since the moisture content of the filter cake cake filter is greater than the OK filter cake water content, when the amount of the circulating washing liquid increases, it can be part of the row.
3.1.2 static washing, recycling and washing 4A zeolite technical conditions:
1. Static washing volume: 1-1.5 times (relative to dry zeolite). Adjust the volume of static washing and control the liquid NT9-10g/l. To prevent filter cake cracking, ensure that the static washing effect.
2, cycle washing L / S: 4
3, circulating cleaning liquid NT: 9-10g/l, NC>NT: 3g/l
4, washing temperature: room temperature
5, CO2 consumption is about 8kg/t-4A, CO2 absorption rate is 20% -30%.
3.2. Industrial expansion test
Table 3 Results of Static Washing, Cyclic Neutralization, and Washing of 4A Zeolite Results
time Recycling lotion Delivery lotion Tape wash CO2 OK moisture Finished product PH Burn off Calcium exchange
Day 1 of the experiment Nt Nc Nt Nt Grand total %
16:30 1.95 3.34 8.5 43.1 4885 28.44 10.9 20.34 303
18:30 5.85 9.5 8.55 43.65 4904 26.1 10.9 19.24 301
20:30 8.45 8.9 19.45 46.05 4910 25.31
22:30 7.9 13.8 20.45 35.65 4925 26.74
Day 2 of the experiment
00:30 7.45 13.1 13.7 32 4936 23.49 10.84 19.82 298
02:30 6.3 10.8 14.7 43.9 4945 23.62
04:30 10.4 13.2 14.85 44.5 4968 25.55 10.82 21.01 298
06:30 12.4 17.2 28.5 41.1 27.75
08:30 12.5 17.4 29.2 22.8 22.36
11:30 12.9 14.8 30.6 33 26.69 10.79 20.54 308
14:30 14.1 11.2 11.7 38.2 4998 21.8
17:30 16.05 12.1 17.6 39.9 27.26 10.84 20.46 309
20:30 5.32 3.74 17.48 39.9 29.91 10.98 20.72 310
23:30 8.72 3.24 19.42 41.5 20.61 11.03 20.65 306
Day 3 of the experiment
02:30 10.3 11.2 19.3 42.2 5043 11.01 20.15 310
05:30 10.2 14.8 32.2 42.15 5058 29.57 11.02 20.68 310
08:30 8.38 10.8 31.4 40.6 5064 25.74
10:30 11.26 8.8 25.28 5071 28.58
14:30 12.3 9.8 17.8 45.4 5079 23.33 10.83 20.28 310
17:30 7.12 6.2 23.62 49.1 5094 23.36
20:30 2.88 2.56 23.6 46.65 5115 29.27
23:30 8.75 6.1 20.3 44.1 5134 24.6
Day 4 of the experiment
02:30 13.05 10.3 21.8 45.7 5149 33.6 10.85 20.33 303
05:30 13.8 13.4 26.45 50.4 5174 29.32 10.82 20.78 307
08:30 14.4 13.4 27.85 44.2 5190 25.89 10.71 20.08 308
11:30 17.4 14.6 27.8 46.95 5208 21.24 10.80 20.59 310
14:30 18.6 14.4 37.9 41.6 5223 21.89
17:30 20.6 8.4 29.6 46.3 5237 23.59 10.81 20.23 307
20:30 7.9 4.9 28.7 42.2 18.86 10.86 20.79 308
23:30 1.9 1 20.8 30.5 23.56 10.84 20.85 310
Day 5 of the experiment
02:30 5.9 5.4 30.6 47.65 5292 20.64 10.86 20.79 308
05:30 7.2 6.04 21.95 45.1 22.64 10.84 20.85 310
08:30 8.6 6.3 17.80 45.5 5318 27.83 10.82 20.24 310
11:30 13.0 7.0 18.40 48.10 5330 20.82
14:30 14.75 6.9 26.8 48.95 18.97 10.87 20.26 306















































Table 4 Record of Samples of 4A Zeolite Produced during Washing Water Test in Production Workshop
Sample lot number Calcium exchange (mg/g) Burn off
(%)
PH BaiDu
(%)
Particle size D50, μm Al3+%
ZP-026050147 309 20.32 11.00 98.0 2.58 18.21
ZP-026050148 309 20.41 10.99 97.9 2.63 18.22
ZP-026050149 309 19.98 11.01 98.2 2.54 18.20
ZP-026050150 308 20.13 11.01 98.2 2.49 18.19
ZP-026050151 309 20.74 10.97 98.1 2.77 18.21
ZP-026050152 308 20.57 10.97 98.0 2.80 18.18
ZP-026050153 309 20.74 10.96 98.0 2.60 18.20
ZP-026050155 309 20.74 10.97 98.0 2.61 18.21
ZP-026050154 309 20.46 10.95 98.1 2.64 18.22
ZP-026050156 309 20.48 10.95 98.1 2.72 18.20
ZP-026050157 308 20.61 10.95 98.0 2.57 18.18
ZP-026050158 309 20.43 10.96 98.1 2.48 18.22
ZP-026050159 308 20.31 10.96 98.1 2.83 18.20
ZP-026050160 309 20.92 10.94 98.0 2.74 18.23
ZP-026050161 308 20.66 10.94 98.0 2.74 18.19
ZP-026050162 309 20.80 10.98 98.0 2.80 18.22
ZP-026050163 309 20.73 10.97 98.1 2.76 18.23
ZP-026050164 309 20.63 10.98 98.0 2.60 18.21
ZP-026050165 308 20.47 10.99 98.0 2.53 18.19









































Table 5 Production Table Unit Consumption Record Table During Industrial Experiment
March 29 Water consumption Steam consumption Yield
5.04 0.98 242.54
March 30 Water consumption Steam consumption Yield
3.95
<, /TD>
0.74 275.7
March 31 Water consumption Steam consumption Yield
2.71 0.687 310

4 Conclusion
Through industrial tests, the conditions worked out in the laboratory were verified. At the same time, some conditions were adjusted in industrial tests. Some problems that occurred in industrial production were solved. From the results:
4.1 Effectively reduce the amount of washing water, saving about 3 tons of washing water consumption, this can be seen from the statistics table of unit consumption;
4.2 The total alkali concentration of the outgoing lotion also reached a suitable level. From the industrial test records, the normal value is about 30g/l or more, which can be reasonably used;
4.3 The quality of the product remains stable, and the product cost is appropriately reduced.
It can be said that this scheme has gone through the process, achieved the effect of saving water and energy, and at the same time reduced the amount of outgoing lotion and realized the expected requirements.


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