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Calcium cyclohexylsulfamate preparation method

A technology of calcium cyclamate and calcium cyclamate, which is applied in the field of preparation of calcium cyclamate to achieve the effects of high conversion rate, easy availability of raw materials, and high stability

Inactive Publication Date: 2016-11-09
JIANGSU LIANWEI BIOCHEM IND CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, driven by profit, calcium cyclamate is often used in excess and beyond the range, especially in children's food, which is easy to be ingested by children in large quantities for a long time

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] A kind of preparation method of calcium cyclamate of the present invention comprises following steps:

[0036](1) Neutralization: Make the cyclohexylamine solution react with sulfamic acid at a pH of 6.8 and below 80°C; set the concentration of the cyclohexylamine solution to 18mg / L, pump the cyclohexylamine solution to 3.5L to neutralize bucket, start the neutralization bucket and stir for 5 minutes, then slowly and evenly add sulfamic acid, and then continue to stir for more than 5 minutes to make the bucket material completely uniform, use a beaker to take 100mL neutralization solution from the sampling port of the neutralization bucket For example, use white phenolphthalein test paper to test its color change. If the color is red, it means that sulfamic acid needs to be added until the test paper does not change color; then adjust the pH value and test it with yellow test paper. If the color is dark blue, add sulfamic acid. If it does not change color, add dilute am...

Embodiment 2

[0056] The difference between embodiment 2 and embodiment 1 is: a kind of preparation method of calcium cyclamate of the present invention comprises following steps:

[0057] In step (1), neutralization: react the cyclohexylamine solution with sulfamic acid at a pH of 6.9 and below 80° C.; pump 4.5 L of the cyclohexylamine solution into the neutralization barrel.

[0058] In step (2), concentration: make the reaction product obtained in step (1) into a state of vacuum concentration and dehydration, start stirring after 2.5 hours of concentration, and concentrate to obtain a concentrated product;

[0059] The concentration process is divided into two stages: the steam pressure in the early stage is 0.20MPa, the temperature is 80°C, and the concentration in the later stage enters the 8-hour period; the concentration process needs to frequently observe the change of the liquid level in the barrel and regularly discharge the accumulated water in the vacuum neutralization barrel. W...

Embodiment 3

[0070] The difference between embodiment 3 and embodiment 1 is: a kind of preparation method of calcium cyclamate of the present invention comprises following steps:

[0071] In step (1), neutralization: react the cyclohexylamine solution with sulfamic acid at a pH of 7.0 and below 80° C.; pump 5.25 L of the cyclohexylamine solution into the neutralization tank.

[0072] In step (2), concentration: make the reaction product obtained in step (1) into a state of vacuum concentration and dehydration, start stirring after 3 hours of concentration, and concentrate to obtain a concentrated product;

[0073] The concentration process is divided into two stages: the steam pressure in the early stage is 0.30MPa, and the temperature is 100°C; the concentration in the later stage enters 14 hours, and the moisture in the material is concentrated and separated. As the liquid level in the barrel gradually decreases, the material becomes thicker and the temperature exceeds For high-efficienc...

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PUM

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Abstract

The invention discloses a calcium cyclohexylsulfamate preparation method, which comprises: (1) neutralizing: carrying out a reaction on cyclohexylamine and aminosulfonic acid at a temperature of less than 80 DEG C under the pH value of 6.8-7.0; (2) concentrating: concentrating the reaction product obtained in the step (1) to obtain a concentrated product, wherein stirring is started after the concentrating is performed for 2-3 h; (3) carrying out a reaction: carrying out a reaction on the concentrated product and cyclohexylamine at a temperature of 60-150 DEG C to obtain a half finished product; (4) recovering: recovering the partial cyclohexylamine, and shortening the decomposition time; (5) adding an alkali: adding calcium hydroxide and water to the half finished product obtained in the step (3), and carrying out a replacement reaction to obtain a product mixture; (6) adjusting: adjusting the product mixture; and (7) crystallizing the adjusted product mixture, and separating to obtain the calcium cyclohexylsulfamate. According to the present invention, the preparation method has characteristics of simple process, easily-available raw materials, low energy consumption, high yield, high product purity, easy use, and high conversion rate.

Description

technical field [0001] The invention relates to the field of food, in particular to a preparation method of calcium cyclamate. Background technique [0002] Calcium cyclamate is a common sweetener whose sweetness is 30-40 times that of sucrose. If consumers often consume beverages or other foods with excessive calcium cyclamate content, excessive intake will cause harm to the human liver and nervous system, especially for the elderly, pregnant women and children who are weak in metabolism and detoxification. The hazards are more obvious. It is formed by reacting sulfamic acid with cyclohexylamine (C6H11NH2) and calcium hydroxide. [0003] Sweetener, white needle, flaky crystal or crystalline powder. Odorless. It tastes sweet, and the sweetness of its dilute solution is about 30 times that of sucrose. The sweetness is 40 to 50 times that of sucrose, and it is a non-nutritive sweetener. 10% aqueous solution is neutral (PH value 6.5), stable to heat, light and air. Sligh...

Claims

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Application Information

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IPC IPC(8): C07C303/34C07C307/02
CPCC07C303/34C07C307/02
Inventor 谢志伟杨华
Owner JIANGSU LIANWEI BIOCHEM IND CO LTD
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