Synthesis of

Thermochromic Materials

Clean, dry, and cool:

(2016/03/04 revised)

Two 50 mL Erlenmeyer flask

Two droppers, one test tube

Collect:
One Styrofoam cup (for ice bath)
One Hirsch funnel (suction filtration)
One rubber stopper (suction filtration)
One suction filtration flask (suction filtration)
One universal clamp

One magnetic stirrer (from TA)

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Objective
Objective
To synthesize a solid with a thermochromic property
from diethylamine hydrochloride and copper (II)
chloride
2(CH3CH2)2NHHCl CuCl2
[(CH3CH2)2NH2]2[CuCl4]
Thermochromic material
Substance that changes color with temperature
Divided into continuously thermochromic and
discontinuously thermochromic two types
This transition is most often due to a change in crystalline
phase, a change in geometry, or a change in the number
of ligands in the coordination sphere

Introduction
[(CH3CH2)2NH2]2 [CuCl4]
Bright green at room temperature
Yellow-brown when temperature increases
The color change is caused by a change in the geometric
orientation of the four ligands around the central copper ion
[CuCl4]2-

[CuCl4]2Low temp.
Square planar, color green

High temp.
Distorted tetrahedron, color brown
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Procedure 1. Prepare Reactants

Clean, dry, cool:

Erlenmeyer flask
Glass dropper
Test tube

*All glassware used must be dry

Weigh 0.005 mol CuCl2 (0.70 g )

Dissolve with 2 mL absolute
ethanol

0.01 mol diethylamine

hydrochloride (1.10 g)
Add 6 mL isopropyl
alcohol
Heat at low temp. to
dissolve
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Procedure 2. Synthesize Product

Keep stirring
Add copper(II) chloride
solution by drop to the
diethylamine hydrochloride
Observe color change

In fume hood
Heat and stir to evaporate the excess
solvent
Heat until ca. 4 mL (compare with 4
mL of water)
Remove magnetic stirring bar
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Procedure 3.
Produce Crystalline Solid

Stay cool
Place in ice-water
bath for
crystallization

Scrape wall of flask

with glass rod to
invoke
crystallization

Add 6 mL ice-cold
isopropyl alcohol
Break up solids with
glass rod and rinse
precipitate

Procedure 4. Suction
Filtration to Collect Product
Suction filtration

Suction filtration to collect product

Use Hirsch funnel

Fix filtration flask and vacuum
flask with extension clamp
Place a rubber stopper between
suction flask and funnel
Rinse filter paper with small
amounts of solvent
Close the two-way valve and
start suction
Start filtering when the filter
paper is tightly stuck on the
funnel
Remaining solution should
placed back into ice-water bath
to keep cool

Procedure 5. Pack the Product

into Capillary Tube (Method 1)

Take a capillary tube that is sealed on one end

Stuff the opening end with the crystalline product

Clean the outer walls of the capillary tube

Drop the capillary tube in a long glass pipe (or funnel) so that
it strikes the table top

Product will be compacted into the sealed end of the tube

Seal capillary tube with gas burner

Procedure 5. Pack the Product

into Capillary Tube (Method 2)

Take a capillary tube with two open ends

Stuff one end of the capillary tube with the crystalline product

Wipe clean the outer wall of the capillary tube

Apply vacuum to capillary tube to suck the product to the center of

capillary tube

Seal both ends of capillary tube with gas burner

Procedure 6. Determining the

Thermochromic Temperature

Observe the temp. range

of color change

Fix capillary tube with

thermometer (with blank label or
tape)

Place into 100 mL beaker of cold

water

Start heating to observe color

change and temperature

Place back into ice bath

Observe if the color change is

irreversible
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Notice

Both of the reactants are hygroscopic, seal cap after use

If the product is stuck on the long glass tube, clean the tube with water
immediately and place it in oven to dry

If the product cannot be properly stuffed into a capillary tube, small

amounts can be transferred into a test tube. Stopper the test tube and
put into ice bath to observe color change

The gas burners are operated under the supervision of TA

The thermochromic capillary tube can be taken home as a souvenir

Discard unwanted capillary tube into designated recycling point

Waste materials contain heavy metals and must be recycled

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