CN103570592A - Acesulfame synthesis and acylation production process - Google Patents

Abstract

The invention relates to an acesulfame synthesis and acylation production process, which comprises the following steps of a, putting a sulfamic acid and dichloromethane into a dissolving kettle, and pumping a mixture into a synthesis kettle; b, adding dropwise triethylamine into the synthesis kettle, adding dropwise a glacial acetic acid, and performing natural reaction for 1 hour after the glacial acetic acid is added dropwise; c, placing reactants in the synthesis kettle into an acylation kettle, and adding dropwise diketene for an acylation reaction; and d, after the diketene is added dropwise, circulating a product subjected to the acylation reaction for 1 hour in the acylation kettle, placing into a heat-preservation kettle, performing natural reaction for 1 hour to generate an acetoacetyl-N-sulfonate intermediate, and feeding the acetoacetyl-N-sulfonate intermediate to a sulfonation section for use. The acesulfame synthesis and acylation production process has the advantages that 1, a stepwise reaction mode is adopted, so that compared with a conventional single-kettle production process, the method has the characteristics of production operation continuity and high reaction stability; 2, a multi-kettle stepwise production mode is adopted, so that the production efficiency is greatly improved, the reaction efficiency of the whole production flow is optimized, and the economic benefits of an enterprise are significantly improved.

Description

Acesulfame potassium synthesizes acylation production process

Technical field:

The present invention relates to a kind of acesulfame potassium synthetic acidylate workshop section production method in producing.

Background technology:

In traditional acesulfame potassium production technique, as shown in Figure 1, various raw materials add respectively synthesis reactor according to dosage to synthesizing section, and institute responds and all in same reactor, carries out, and the technological reaction time is long, and production capacity is low, low conversion rate, and by product is many, and production cost is high.

Summary of the invention:

Object of the present invention is exactly that long reaction time, production capacity that a still reaction exists are low in order to overcome in existing use technology, low conversion rate, shortcoming that by product is many, a kind of acesulfame potassium substep production acylation reaction technique providing.

To achieve these goals, the present invention has adopted following technical scheme:

1, the synthetic acylation production process of acesulfame potassium, is characterized in that comprising the following steps:

A, by dosage, thionamic acid and methylene dichloride are squeezed into respectively in molten material still and mixed, mixture pump is to synthesis reactor;

B, pacify dosage first drip triethylamine in synthesis reactor, flow is at 400L-800L/h, and dropping temperature is at 10-25 ℃; After dropping triethylamine is complete, by dosage, drip Glacial acetic acid again, flow 10L/min, temperature, at 10-25 ℃, drips after Glacial acetic acid, natural reaction 1 hour;

Reactant in c, synthesis reactor is put into acidylate still, drips two rare ketone of second carry out acylation reaction by dosage, and the rare ketone of two second drips flow 200-250L/h, and acidylate still temperature is at 15-25 ℃;

After d, the rare ketone of two second drip and finishes, circulate 1 hour in acidylate still, then put into insulation still and carry out natural reaction 1 hour, after natural reaction, temperature is down to 0-5 ℃, generates acetoacetyl-N-sulfonate intermediate, sends into sulfonation workshop section and uses.

Each raw material adopting in technique scheme, in all producing according to acesulfame potassium, known ratio of components is prepared burden.

Advantage of the present invention:

1, adopt stepwise reaction technique, realize the continuity of production operation, reduced labor strength.

2, original traditional single still production technique, stepwise reaction stability is high, improves reactor work-ing life, alleviates deep cooling load.

3, production efficiency increases substantially, and traditional technology list still drips all raw materials, and error in dipping is larger, reaction efficiency is low, and material waste is serious, utilizes now many stills to produce step by step, make whole Production Flow Chart realization response efficiency optimization, obviously increased Business Economic Benefit.

4, this technique rational proportion material, can effectively reduce foreign matter content in finished product, improves product quality.

5, by improving acylation reaction temperature, promote acylation reaction transformation efficiency, simultaneously Reaction time shorten.

Accompanying drawing explanation:

Fig. 1 is synthesizing section schema in existing acesulfame potassium production technique;

Fig. 2 is synthesizing section schema in acesulfame potassium production technique of the present invention.

Embodiment

Embodiment 1, as shown in Figure 2:

One. accurate feed proportioning 3325kg(2500L) methylene dichloride, open methylene dichloride scale tank valve and add methylene dichloride 2000L in dry molten material still, start and stir and recycle pump; From batching hole, drop into thionamic acid 1000kg.Close circulation valve, open feeding valve, mixture in molten material still is delivered in dry synthesis reactor.After feeding finishes, by remaining 500L methylene dichloride in scale tank, put into molten material still, after circulation, send in synthesis reactor that (methylene dichloride just mixes together with thionamic acid, without chemical reaction, so rinse remaining thionamic acid in molten material still with 500L methylene dichloride, guarantee that blending process is accurate at normal temperature.The process that molten material still feeds intake is to carry out at normal temperatures).

Two. open salt water for cooling, below still still temperature drop to 15 to be synthesized ℃, during accurate feed proportioning triethylamine 1550L(batching, check and to synthesis reactor, put triethylamine valve and all keep closing), then evenly drip triethylamine; Flow is at 400L-800L/h.

Three. synthesis reactor temperature is 25 ℃ of left and right, and when triethylamine drips end, by PH detection paper material pH value, the micro-aobvious light green of test paper, pH value is between 7.5-9, and still temperature to be synthesized is adjusted to normal temperature (10-25 ℃) natural reaction 1 hour;

Four. drip Glacial acetic acid 50kg, flow 10L/min, drips and finishes, and opens salt water for cooling, naturally puts and answers 1 hour, maintains the temperature at 10-25 ℃.

Five. after synthesis reactor natural reaction finishes, material is put into acidylate still, open salt solution and be cooled to 10 ℃.Accurately take 920kg(845L) ketene dimer, open dropping valve, evenly drip ketene dimer, flow 200-250L/h, maintains the temperature at 15-25 ℃.

Six. ketene dimer drips and finishes, and regulates acidylate still temperature to 20-25 ℃, then puts into insulation still, natural reaction 1 hour, temperature is down to 0-5 ℃, generates acetoacetyl-N-sulfonate intermediate content >=40%, can send into sulfonation post and use.

Claims (1)

1. acesulfame potassium synthesizes acylation production process, it is characterized in that comprising the following steps:

A, by dosage, thionamic acid and methylene dichloride are squeezed into respectively in molten material still and mixed, mixture pump is to synthesis reactor;

B, in synthesis reactor, by dosage, first drip triethylamine, drip flow at 400L-800L/h, dropping temperature is at 10-25 ℃; After dropping triethylamine is complete, drip Glacial acetic acid again by dosage, drip flow 10L/min, temperature, at 10-25 ℃, drips after Glacial acetic acid, natural reaction 1 hour;

Reactant in c, synthesis reactor is put into acidylate still, drips two rare ketone of second carry out acylation reaction by dosage, and the rare ketone of two second drips flow 200-250L/h, and acidylate still temperature is at 15-25 ℃;

After d, the rare ketone of two second drip and finishes, circulate 1 hour in acidylate still, then put into insulation still and carry out natural reaction 1 hour, after natural reaction, temperature is down to 0-5 ℃, generates acetoacetyl-N-sulfonate intermediate, sends into sulfonation workshop section and uses.

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